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Method for separating amide from amino acid ionic liquid

An ionic liquid and amino acid technology, which is applied in the field of separating amides from amino acid ionic liquids, can solve the problems of separating product caprolactam, etc., and achieve the effect of high ketoxime rearrangement reaction conversion rate and amide selectivity.

Inactive Publication Date: 2013-03-27
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most important reason is that the product caprolactam cannot be separated from the rearrangement reaction system, that is, the separation of amides from the liquid-phase Beckmann rearrangement reaction system is the main obstacle to the development of ammonium sulfate-free by-product reactions.

Method used

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  • Method for separating amide from amino acid ionic liquid
  • Method for separating amide from amino acid ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1-9

[0037] In embodiment 1 to 9, be to add 100 milliliters of toluene solvents and 0.01 mole of glutamic acid sulfuric acid type ionic liquid containing the sulfuric acid that the molar concentration exceeds one times in the three-neck round bottom flask of 250 milliliters, and stir with magnet and be warming up to After 110°C, add 0.002 mole of cyclohexanone oxime, and the molar ratio of ionic liquid to ketoxime is 5:1. After the reaction was carried out for 0.5 hours, after it was cooled to remove the toluene phase, 15 grams of water and 7.42 grams of the extractant listed in Table 1 were added, stirred at 60° C. for 5 minutes, placed in a separatory funnel for static separation, and collected For the extractant phase, repeat the above extraction steps twice, collect the extractant phase and analyze it with a gas chromatograph, and then extract the ionic liquid phase with chloroform, 30 ml each time, and monitor with a gas chromatograph until almost no caprolactam remains in the ...

Embodiment 10-14

[0047] In embodiment 10 to 14, be to add 150 milliliters of toluene solvents and 0.05 mole of the glutamic acid sulfuric acid type ionic liquid containing the sulfuric acid of molar concentration excess in the three-neck round-bottomed flask of 250 milliliters, and stir with magnet and be warming up to After 110°C, 0.03 mole of cyclohexanone oxime was added, and the molar ratio of ionic liquid to ketoxime was 5:3. After the reaction was carried out for 0.5 hours, the toluene phase was removed after it was cooled, and water and 37.10 grams of 2-tert-butylphenol were added according to the records in Table 3, stirred at 60°C for 5 minutes, and placed in a separatory funnel for static separation. layer, collect the extractant phase, analyze it with a gas chromatograph, and then extract the ionic liquid phase with chloroform, each 30 milliliters, monitor with a gas chromatograph until almost no caprolactam remains in the ionic liquid, the conversion rate of the reactant and The se...

Embodiment 15-19

[0055] In embodiment 15 to 19, be to add 150 milliliters of toluene solvents and 0.05 mole of the glutamic acid sulfuric acid type ionic liquid containing the sulfuric acid of molar concentration excess in the three-neck round bottom flask of 250 milliliters, and stir with magnet and be warming up to After 110°C, 0.01, 0.02, 0.03, 0.04, 0.05 moles of cyclohexanone oxime were added respectively, and the molar ratio of ionic liquid and ketoxime is shown in Table 4. After the reaction was carried out for 0.5 hours, after cooling to remove the toluene phase, add 9.28 grams of water and 37.10 grams of 2-tert-butylphenol, stir at 60°C for 5 minutes, put it in a separatory funnel and let it stand to separate layers, and collect the extractant Phase, repeat the above extraction steps twice, collect the extractant phase and analyze it with a gas chromatograph, and then extract the ionic liquid phase with chloroform, 30 ml each time, monitor with a gas chromatograph until almost no capro...

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Abstract

The invention discloses a method for separating amide from amino acid ionic liquid, which comprises the following steps of: adding a polar solvent and an extractant into the amino acid ionic liquid; and separating out the amide from the amino acid ionic liquid. The method has the advantages that: ammonia water is not needed to be added and an ammonium sulfate byproduct is not generated in an extraction stage; moreover, after the amide is separated from the ionic liquid, the ionic liquid can be recycled, and the like.

Description

technical field [0001] The invention relates to a method for separating amides, in particular to a method for separating amides from amino acid ionic liquids. Background technique [0002] Caprolactam is an important raw material for the manufacture of nylon 6 fibers and films. The Beckmann rearrangement reaction of cyclohexanone oxime is the most important reaction step in the production of caprolactam. At present, the traditional rearrangement reaction process uses oleum (Oleum) as a catalyst to produce cyclohexanone oxime through liquid-phase Beckmann rearrangement reaction. Caprolactam sulfate, and then neutralized with ammonia water to obtain caprolactam. Although the conversion rate of cyclohexanone oxime in the whole reaction is almost 100%, and the selectivity of caprolactam is 99%, the whole reaction not only produces a large amount of low-value ammonium sulfate, but also the catalyzed concentrated sulfuric acid causes corrosion and environmental pollution to the w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D201/16C07D201/04C07D223/10
Inventor 谢正发施建全陈启元
Owner CHINA PETROCHEM DEVMENT