Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Purification method of ethyl acetate for liquid chromatography-mass spectrometer

A technology of ethyl acetate and liquid chromatography, applied in the separation/purification of carboxylate, chemical instruments and methods, preparation of carboxylate, etc. To solve problems such as instrumentation, to achieve the effect of simple production process, filling the gap in production, and expanding the scope of application

Active Publication Date: 2015-11-25
上海星可高纯溶剂有限公司
View PDF6 Cites 2 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Purification method of ethyl acetate for liquid chromatography-mass spectrometer
  • Purification method of ethyl acetate for liquid chromatography-mass spectrometer

Examples

Experimental program
Comparison scheme
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 distilled ethyl acetate to adjust the pH of the solution to 8, and shake to make potassium ...

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle size (mesh)aaaaaaaaaa
particle diameteraaaaaaaaaa
particle size (mesh)aaaaaaaaaa
Login to View More

Abstract

The invention discloses a purification method of ethyl acetate for a liquid chromatography-mass spectrometer. The method is characterized in that impurities in a raw material ethyl acetate are removed through processes such as modified active carbon adsorption and the like so as to obtain ethyl acetate for a liquid chromatography-mass spectrometer. By the purification method of ethyl acetate for a liquid chromatography-mass spectrometer, ethyl acetate with purity being greater than or equal to 99.99 wt% can be obtained. The method meets high-purity requirement of a liquid chromatography-mass spectrometer. Therefore, ethyl acetate obtained after purification can be applied in the field of liquid chromatography-mass spectrometers, and the application range of ethyl acetate is broadened.

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 Chromatography Mass Spectrometer (LC-MS for short) is a high-end instrument in the organic analysis market. Liquid chromatography (LC) can effectivel...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com