Ethylene carbonate continuous melt crystallization device and method

A technology of ethylene carbonate and melt crystallization, which is applied in the directions of crystallization separation, solution crystallization, and crystallization condition screening, etc., can solve the problems that cannot reflect the energy-saving advantages of the crystallization process, unstable product quality, low production efficiency, etc., and achieve structural Compactness, reduced need to sweat, high productivity

Active Publication Date: 2021-04-27
天津乐科节能科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been related patent reports on the separation and purification of ethylene carbonate by melting crystallization, such as Japanese patent document JP-7-89905 and Chinese patent CN201811248553.3, but most of them are intermittent operations, which have low production efficiency, high labor intensity, and need to change jobs Condition control, unstable product quality and other issues
At the same time, since the intermittent process needs to continuously switch between hot and cold media for temperature rise and fall, a large part of energy consumption is wasted, which cannot well reflect the energy-saving advantages of the crystallization process

Method used

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  • Ethylene carbonate continuous melt crystallization device and method
  • Ethylene carbonate continuous melt crystallization device and method
  • Ethylene carbonate continuous melt crystallization device and method

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Experimental program
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Effect test

Embodiment 1

[0038]A ethylene carbonate continuous melting and crystallization equipment is a vertical structure, which is divided into a crystallization area, a crystal bed area and a melting area from top to bottom along the axial direction. The diameter of the equipment is 800mm, the height of the crystallization area is 4000mm, and the height of the crystal bed area is 1500mm , The height of the melting zone is 800mm. Heat exchange fins A and heat exchange fins B are alternately arranged in the crystallization area, and reinforcing ribs are provided inside the heat exchange fins to form a cooling fluid flow channel, and the adjacent heat exchange fins are connected in series. A vertical scraper is arranged between two adjacent heat exchange fins. The top of the heat exchange fin A corresponds to a group of scrapers. The plane of the scraper is perpendicular to the plane of the heat exchange fin and forms an angle of 45 degrees with the connecting rod. When rotating, the scraper pushes t...

Embodiment 2

[0040] Using the pilot equipment listed in Example 1, the superior grade ethylene carbonate with 99.9wt% purity (remaining part is ethylene glycol and other impurities) is a raw material for continuous melting crystallization experiment, the feed flow rate is 1500kg / h, and the feed temperature is 40 ℃, control the flow rate of circulating cooling water and the flow rate of low-pressure steam in the melting zone, so that the discharge rate is 1200kg / h, the overflow rate of the mother liquor is 300kg / h, and the height of the crystal bed can be kept stable, and at the same time, the cold and heat can meet the needs of the melting zone. After the inner crystal melts, the liquid phase reflux ratio is 3. At this time, the heat transfer temperature difference in the crystallization zone is 15°C, and the heat transfer temperature difference in the melting zone is 60°C. After the equipment was running stably for 10 hours, a sample was taken and analyzed. The purity of the product was 99...

Embodiment 3

[0042] Using the pilot equipment listed in Example 1, industrial-grade ethylene carbonate with a purity of 99.5wt% (remaining part is ethylene glycol and other impurities) is used as a raw material for continuous melting and crystallization experiments, and the feed flow rate is controlled to be 1500kg / h. 40°C, control the flow rate of circulating cooling water and the flow rate of low-pressure steam in the melting zone, so that the discharge rate is 720kg / h, the overflow rate of the mother liquor is 780kg / h, and the height of the crystal bed can be kept stable, while the cold heat can meet the requirements of melting The reflux ratio of the liquid phase in the zone is 5 after the crystal melts. At this time, the heat transfer temperature difference in the crystallization zone is 9°C, and the heat transfer temperature difference in the melting zone is 35°C. After the equipment was running stably for 10 hours, sampling and analysis showed that the product had a purity of 99.995w...

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Abstract

The invention discloses an ethylene carbonate continuous melt crystallization device and a method, the device is a vertical structure, and is divided into a crystallization zone, a crystal bed zone and a melting zone along the axial direction of the device, the crystallization zone is internally provided with a heat exchange sheet and a stirring scraper for cooling crystallization of an ethylene carbonate stock solution, crystals settle downwards to enter a crystal bed layer section under the action of gravity and machinery and are accumulated to form a crystal bed with a certain height, a heat exchange piece is arranged in a melting area and used for providing heat needed by crystal melting, one part of molten liquid is discharged from a discharging port in the bottom of crystallization equipment, and the other part of the molten liquid axially penetrates through the crystal bed layer to flow upwards in a countercurrent mode. Due to the fact that the high-purity molten liquid carries heat, heat and mass transfer occurs between the high-purity molten liquid and ethylene carbonate crystals in the crystal bed layer during countercurrent, and the sweating process of ethylene carbonate is achieved. The continuous melt crystallization device and method can be used for preparing electronic grade ethylene carbonate, and have the advantages of being high in product purity, high in production efficiency, compact in equipment structure, low in energy consumption, capable of continuously and stably operating and the like.

Description

technical field [0001] The invention belongs to the field of crystallization and purification, in particular to a continuous melting crystallization device and method for ethylene carbonate. Background technique [0002] Ethylene carbonate is a polar high-boiling solvent with good performance, and it can also be used as a surfactant raw material and an organic synthesis intermediate. It is widely used in the field of organic synthesis, for example, furazolidone, dimethyl carbonate, ethylene glycol, functional polymer materials, etc. can be further produced by using ethylene carbonate as raw material. At the same time, ethylene carbonate can also be used for polymer modification. A very important chemical basic raw material. In recent years, with the rapid development of the new energy field, the demand for ethylene carbonate as a battery electrolyte has continued to increase, and the market has continued to expand. At the same time, higher requirements have been placed on t...

Claims

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Application Information

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IPC IPC(8): B01D9/02C07D317/38
CPCB01D9/0013B01D9/0063B01D9/0077B01D2009/0086C07D317/38
Inventor 夏君君于会满彭涛尹海蛟全晓宇唐昊刘莉
Owner 天津乐科节能科技有限公司
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