Method for adopting melting crystallization technology to separate and purify succinonitrile

A technology of melting crystallization and purification method, which is applied in the direction of carboxylic acid nitrile purification/separation, organic chemistry, etc., can solve the problems of complex operation, high energy consumption, polymerization coking, etc., and achieves no influence on yield and quality, low operating temperature, The effect of high product purity

Inactive Publication Date: 2018-02-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Purification of succinonitrile by crystallization needs to consume a large amount of solvent, and the requirement for the purity of the solvent is relatively high. It needs to be a high-purity solvent and consumes a lot of energy; the purification of succinonitrile by adsorption method has a purity of less than 99.95% after purification of succinonitrile, and the adsorption purification The process has strict requirements on the adsorbent, the adsorb

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 52.0°C at a rate of 0.01°C / min, take out the bottom stopper after stabilizing for 180 minutes and release it as the crystallization mother liquor until the liquid is no longer Outflow; then start to heat up and sweat at a rate of 0.01°C / min to 55.0°C, and keep it for 10 minutes, then receive the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 40.1%, and the product purity reaches 99.96%.

Embodiment 2

[0025] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 51.0°C at a rate of 0.005°C / min, take out the bottom plug after stabilization for 120 minutes and release it as a crystallization mother liquor until the liquid is no longer Flow out; then start to heat up and sweat at a rate of 0.05°C / min to 56.0°C, and keep it for 30 minutes, then pick up the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 45.6%, and the product purity reaches 99.97%.

Embodiment 3

[0027] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 50.0°C at a rate of 0.008°C / min, take out the bottom stopper after 60 minutes of stabilization and release it as the crystallization mother liquor until the liquid is no longer Flow out; then start to heat up and sweat at a rate of 0.1°C / min to 57.0°C, and keep it for 60 minutes, then receive the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 45.6%, and the product purity reaches 99.97%.

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Abstract

The invention relates to a method for adopting a melting crystallization technology to separate and purify succinonitrile. According to the method, succinonitrile coarse products are added into a melting crystallizer and heated to 59 DEG C for complete dissolution, then programmed heating is started to raise the temperature to 45-52 DEG C, after the temperature is stabilized for 10-180 min, crystallization mother liquor is released, and succinonitrile coarse crystals are obtained; then programmed heating is started, sweating is conducted, the temperature is stabilized for 10-180 min after reaching final sweating temperature, and high-purity succinonitrilee crystals with the purity of 99.95% or above are obtained. According to the method, a separation method of melting crystallization is adopted, no solvents or vacuum drying is needed, and the operation time is short; the operation is simple, the method is environmentally friendly, the product purity is high, and the crystallization mother liquor and sweating liquid can be recycled and purified again through melting crystallization; compared with an existing decompression batch distillation method, the energy consumption, operatingtemperature and cost are low, no polymerization coking phenomena occur in the operating process, and the yield and quality are not affected.

Description

Technical field [0001] The invention belongs to the technical field of succinonitrile production for lithium ion batteries, and specifically relates to a method for separating and purifying succinonitrile by using a melt crystallization technology. Background technique [0002] The rapid development of the electronics industry has enabled us to enter the era of informationization and digitalization, which has led to an increasing demand for electronic products, which has also made our demand for lithium-ion batteries increase year by year. Bridgestone of Japan developed the first-generation electrolyte additive for lithium-ion batteries in 2002. This additive partially improved the high-temperature performance, cycle performance and safety performance of lithium-ion batteries, and laid the foundation for this. Lithium-ion battery electrolyte additives have the characteristics of strong pertinence and low dosage, which can significantly improve the performance of the battery witho...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C255/04
CPCC07C253/34C07C255/04
Inventor 唐忠利王冬冬王启纶
Owner TIANJIN UNIV
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