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High-purity vinylene carbonate and a method of purifying vinylene carbonate

A vinylene carbonate, high-purity technology, applied in organic chemistry and other fields, can solve the problems of ambiguous purity data and no detailed disclosure

Inactive Publication Date: 2008-05-07
SALTIGO GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0032] It should be noted that in this literature, the analytical method to determine the purity is not disclosed in detail, so the purity data are ambiguous

Method used

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  • High-purity vinylene carbonate and a method of purifying vinylene carbonate

Examples

Experimental program
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example 1

[0064] The purification of example 1 VC:

[0065] Only crude VC substantially free of polymeric impurities by initial distillation without a (distillation) column was used as starting material.

[0066] The purity of this crude VC is about 97% and the content of organic and inorganic chlorine is about 0.5% to 1%.

[0067] Gas chromatography analysis was performed by HP6890. Separation was performed by a 50 meter long CP-Sil 8 CB with 0.53 mm ID and 1.0 μm FD.

[0068] The carrier gas was nitrogen with an inlet pressure of 5 psi. The syringe was operated at a flow rate of 138 ml / min with a 30 / 1 split. Inject 1 μl of pure VC.

[0069] The injector temperature was 220°C and the monitor temperature was 320°C. The temperature program starts at 50°C and heats up to 250°C at 5°C / min.

[0070] Evaluations were performed according to the standard percentage method.

[0071] First processing stage: Treat with urea at 140°C, filter out with air suction, dilute with NMP:

[0072] ...

example 2

[0091] The characteristic comparison of example 2 liquid VC and solid VC

[0092] Samples of vinylene carbonate purified according to Example 1 were stored in liquid state at 20° C. and in crystalline form at 5° C. without stabilizers and protected from light.

[0093] Liquid VC

[0094] The stabilizer-free vinylene carbonate sample exhibited mild to severe yellow discoloration and slight clouding after 70 days. The content was mostly 96% as measured by ISTD. Liquid, high-purity vinylene carbonate is storage-unstable in the absence of a stabilizer.

[0095] Solid VC

[0096] The solid samples stored at 5°C were all colorless and clear even after 365 days, after melting. Analysis showed no change in mass. Vinylene carbonate without stabilizer is stable in solid state storage.

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Abstract

The present invention relates to the industrial purification of vinylene carbonate by simple thermal treatment of organics with amide nitrogen-hydrogen bonds, followed by distillation and melt crystallization. VC of extremely high purity is obtained in this way. This high-purity vinylene carbonate can be stored and transported without stabilizers.

Description

technical field [0001] The present invention relates to solid-state aggregated high-purity vinylene carbonate (VC) and a method for purifying vinylene carbonate. Vinylene carbonate is an important intermediate used in the production of chemicals, pharmaceutical products, crop protection agents, especially in polymers, coatings and battery electrolytes. Background technique [0002] Vinylene carbonate is produced by known methods of eliminating hydrogen chloride from chloroethylene carbonate with tertiary amines, especially triethylamine. [0003] Chloroethylene carbonate is obtained by free radical chlorination of ethylene carbonate using chlorine or sulfuryl chloride. [0004] This synthetic method was first published by Newman and Addor in 1953 (JACS, 1953, P1263; JACS 1955, P3789). [0005] Glycol carbonate (GC) itself is photochlorinated using UV light at 60-70°C, and the resulting CGC is purified by vacuum distillation. [0006] Newman and Addor obtained VC by using ...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 赖因哈特·朗格尔保尔·瓦格纳海因里希·格日尼亚
Owner SALTIGO GMBH
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