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Purification method of ethyl acetate for liquid chromatography-mass spectrometry

A technology of ethyl acetate and liquid chromatography, applied in the separation/purification of carboxylate, chemical instruments and methods, preparation of carboxylate, etc. Problems such as the use of instruments, to achieve the effect of simple production process, filling production gaps, and low energy consumption

Active Publication Date: 2018-04-24
上海星可高纯溶剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, the progress of the esterification reaction will be accompanied by the generation of side reactions to generate by-products such as ether and ethylene.
Residual reactants and by-products will cause the purity of ethyl acetate to decrease, and the purity of industrial grade ethyl acetate is generally not higher than 95%, which cannot meet the requirements of liquid chromatography-mass spectrometry

Method used

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  • Purification method of ethyl acetate for liquid chromatography-mass spectrometry
  • Purification method of ethyl acetate for liquid chromatography-mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The purification method of ethyl acetate for liquid chromatography-mass spectrometry, is characterized in that, comprises the steps:

[0024] a. Take the raw material ethyl acetate, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetonitrile Impurities such as amides. Add high manganese

[0025] At the same time as potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 8. After the oxidation treatment, the ethyl acetate was quickly distilled off.

[0026] a'. Will add reducing agent ferrous oxide and stir in the ethyl acetate gained in step a, distill out ethyl acetate.

[0027] b. Add sodium carbonate to the distilled ethyl acetate to adjust the pH of the solution to 7, and s...

Embodiment 2

[0034] The purification method of ethyl acetate for liquid chromatography-mass spectrometry, is characterized in that, comprises the steps:

[0035] a. Take the raw material ethyl acetate, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetonitrile Impurities such as amides. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 14. After the oxidation treatment, the ethyl acetate was quickly distilled off.

[0036] a'. Will add reducing agent sodium bisulfate and stir in the ethyl acetate gained in step a, distill out ethyl acetate.

[0037] b. Add potassium hydroxide to the above-mentioned distilled ethyl acetate to adjust the pH of the solution to 8, and shake to make ...

Embodiment 3

[0044] The purification method of ethyl acetate for liquid chromatography-mass spectrometry, is characterized in that, comprises the steps:

[0045] a. Take the raw material ethyl acetate, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetonitrile Impurities such as amides. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 10. After the oxidation treatment, the ethyl acetate was quickly distilled off.

[0046] a'. Will add reducing agent disodium hydrogen phosphate and stir in the ethyl acetate gained in step a, distill out ethyl acetate.

[0047] b. Add sodium oxide to the above-mentioned distilled ethyl acetate to adjust the pH of the solution to 7.5, and shake to...

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Abstract

The invention discloses a method for purifying ethyl acetate for liquid chromatography-mass spectrometry, which is characterized in that impurities in raw ethyl acetate are removed through procedures such as modified activated carbon adsorption to obtain liquid chromatography-mass spectrometry. Use ethyl acetate. The liquid chromatography-mass spectrometry purification method provided by the invention uses ethyl acetate, which can obtain ethyl acetate with a purity ≥ 99.99% (wt), which meets the high purity requirements of the liquid chromatography-mass spectrometry and makes the purification The obtained ethyl acetate can be applied to the field of liquid chromatography-mass spectrometry, which expands the scope of application.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying ethyl acetate for liquid chromatography-mass spectrometry. Background technique [0002] The online coupling of chromatography-mass spectrometry combines the separation ability of chromatography with the qualitative function of mass spectrometry to achieve more accurate quantitative and qualitative analysis of complex mixtures. It also simplifies the pretreatment process of the sample and makes the sample analysis easier. Chromatography-mass spectrometry includes gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry. Liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry complement each other to analyze compounds of different properties. [0003] Liquid Chromatograph Mass Spectrometer (LC-MS for short) is a high-end instrument in the organic analysis market. Liquid chromatography (LC) can effectively...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/48C07C67/56C07C67/60
Inventor 范文林张群星王洪
Owner 上海星可高纯溶剂有限公司
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