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Preparation method and preparation device of electronic-grade dimethyl carbonate

A dimethyl carbonate and preparation device technology, applied in the purification/separation of carbonate/haloformate, general layout of crystallization device, crystallization adjustment/control, etc., can solve high energy consumption and reduce process safety To achieve the effects of high product purity, low energy consumption per unit product, and insensitivity to fluctuations in raw materials

Pending Publication Date: 2022-01-18
德艾柯工业技术(江苏)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this patent, the T1 light removal tower needs a reflux ratio of 30-50, and the energy consumption is high; the T2 pressurized tower is operated at a very high pressure, which increases equipment investment and reduces the safety of the process

Method used

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  • Preparation method and preparation device of electronic-grade dimethyl carbonate

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preparation example Construction

[0065] A kind of preparation method and device of electronic grade dimethyl carbonate, such as figure 1 As shown, the crude DMC product containing 95-99.5 wt% DMC is first stored in the raw material tank 51, and then pumped into the suspension crystallizer 1 for suspension crystallization. Suspension crystallization uses ethylene glycol aqueous solution as a refrigerant (cooling medium), enters the jacket of the suspension crystallizer 1, and controls the temperature of the materials in the suspension crystallizer 1. The material temperature in the suspension crystallizer 1 is set at -5~3.5°C, preferably -4~3°C, more preferably -3.5~2.8°C; the stirring speed is set at 10~30rpm, preferably 15~25rpm, more preferably 18°C ~25rpm; the temperature difference between the inlet temperature of the refrigerant and the material temperature in the suspension crystallizer 1 is 4~15°C, preferably 6~13°C, more preferably 7~12°C; the temperature difference between the inlet and outlet of the...

Embodiment 1

[0073] Using dimethyl carbonate produced by a certain process as a raw material, the content of dimethyl carbonate is 99.5wt%, the moisture content is 460ppm, and the methanol content is 0.4wt%. The remaining components are easily separated components, which are not listed here. .

[0074] Above-mentioned raw material first enters in suspension crystallizer 1 and carries out cooling crystallization, and crystallization material temperature is-2 ℃, and the stirring speed in suspension crystallizer 1 is 22rpm, and the inlet temperature of ethylene glycol aqueous solution in the suspension crystallizer 1 jacket is-8.3 ℃, The temperature difference between the ethylene glycol aqueous solution entering and leaving the jacket of the suspension crystallizer 1 is 0.5° C., and the solid content in the suspension crystallizer 1 is 31 wt%. Adopt vacuum drum filter (solid-liquid separator 2) to carry out solid-liquid separation to the slurry that is obtained by suspension crystallizer 1, ...

Embodiment 2

[0079] Dimethyl carbonate produced by a certain process is used as raw material, wherein the content of dimethyl carbonate is 95.7wt%, the moisture content is 0.7wt%, the methanol content is 2.9wt%, and the remaining components are easily separated components, which are not listed here. listed.

[0080] Above-mentioned raw material first enters in suspension crystallizer 1 and carries out cooling crystallization, and crystallization material temperature is-3 ℃, and the stirring speed in suspension crystallizer 1 is 20rpm, and the inlet temperature of ethylene glycol aqueous solution in suspension crystallizer 1 jacket is-13 ℃, The temperature difference between the ethylene glycol aqueous solution entering and leaving the jacket of the suspension crystallizer 1 is 0.6° C., and the solid content in the suspension crystallizer 1 is 29.6 wt%. Adopt horizontal multistage pusher centrifuge (solid-liquid separator 2) to carry out solid-liquid separation to the slurry that is obtaine...

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Abstract

The invention relates to the field of lithium battery electrolyte, in particular to a preparation method and a preparation device of electronic-grade dimethyl carbonate, and the preparation device comprises a suspension crystallizer, a solid-liquid separator, a static crystallizer and a dehydrating tower; the suspension crystallizer is connected with the dehydrating tower through the solid-liquid separator and the static crystallizer in sequence; and suspension crystallization, solid-liquid separation, static crystallization and dehydration are performed on the crude DMC product to obtain the electronic-grade DMC. Compared with the prior art, the DMC crude product is purified by combining suspension crystallization and static crystallization, aiming at the physical property of the dimethyl carbonate, the process characteristics of the two crystallization modes are fully utilized, the production of the electronic-grade DMC is realized, the methanol content in the product is lower than 20ppm, the water content is lower than 20ppm, and the content of the dimethyl carbonate is not lower than 99.99 wt%; and a plurality of material circulations are set in the process so that the yield of the dimethyl carbonate in the final electronic-grade DMC reaches 80% or above.

Description

technical field [0001] The invention relates to the field of lithium battery electrolyte, in particular to a preparation method and a preparation device of electronic grade dimethyl carbonate. Background technique [0002] In the late 1990s, the rise of green chemistry provided an effective means for mankind to solve the problem of environmental pollution caused by the chemical industry. According to the viewpoint of green chemistry, the root of pollution control should start from the beginning of production, that is, use non-toxic or low-toxic raw materials from the beginning of raw materials, and use production processes that do not produce pollutants as much as possible in production and processes. Under this background, dimethyl carbonate (Dimethyl carbonate, referred to as DMC) has been reborn as a "green intermediate". DMC has very low toxicity, and it was listed as a non-toxic chemical in Europe in 1992. As a new type of green chemical, DMC itself can be produced gr...

Claims

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Application Information

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IPC IPC(8): B01D9/02C07C68/08C07C69/96
CPCB01D9/0059B01D9/0063B01D9/005C07C68/08C07C69/96
Inventor 袁超余圣婴黄婷孙苑洱周叶红
Owner 德艾柯工业技术(江苏)有限公司
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