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Purification method of isopropanol for liquid chromatography-mass spectrometry

A technology of liquid chromatography and purification method, which is applied in the field of purification of isopropanol for liquid chromatography-mass spectrometry, can solve problems such as the inability to meet the high purity requirements of chromatographic grade reagents, and achieve the reduction of import costs and production The effect of simple process and low energy consumption

Active Publication Date: 2018-09-18
上海星可高纯溶剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] There is also a patent for high-purity isopropanol in China. In the patent CN1249294A, a method for refining isopropanol in a combined process of salt extraction and azeotropic distillation is provided. The method adopts the process of extraction and salting out to purify isopropanol. The method It is only a rough purification process, and the purity after purification is >99.5 (wt), which still cannot meet the high purity requirements of chromatographic grade reagents, and the purification method needs to be further improved

Method used

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  • Purification method of isopropanol for liquid chromatography-mass spectrometry

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Effect test

Embodiment 1

[0026] The purification method of isopropanol for liquid chromatography-mass spectrometry is characterized in that, comprises the steps:

[0027] a. Take the raw material isopropanol, 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 8. After the oxidation treatment, the isopropanol is quickly distilled off.

[0028] a'. Will add reducing agent ferrous oxide and stir in the isopropanol gained in step a, distill out isopropanol.

[0029] b. Add sodium carbonate to the distilled isopropanol to adjust the pH of the solution to 7, and shake to make the sodium carbonate fully react with...

Embodiment 2

[0037] The purification method of isopropanol for liquid chromatography-mass spectrometry is characterized in that, comprises the steps:

[0038]a. Take the raw material isopropanol, 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 isopropanol is quickly distilled off.

[0039] a'. Add reducing agent sodium bisulfate and stir in the isopropanol gained in step a, distill out isopropanol.

[0040] b. Add potassium hydroxide to the above-mentioned distilled isopropanol to adjust the pH of the solution to 8, and shake to make potassium hydroxide ...

Embodiment 3

[0048] The purification method of isopropanol for liquid chromatography-mass spectrometry is characterized in that, comprises the steps:

[0049] a. Take the raw material isopropanol, 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 isopropanol is quickly distilled off.

[0050] a'. Add reducing agent disodium hydrogen phosphate to the isopropanol obtained in step a and stir to distill out isopropanol.

[0051] b. Add sodium oxide to the distilled isopropanol to adjust the pH of the solution to 7.5, and shake to make the sodium oxide fully re...

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Abstract

The invention discloses a purification method of isopropyl alcohol for a liquid chromatography-mass spectrometer. The method is characterized in that impurities in a raw material isopropyl alcohol are removed through processes such as modified active carbon adsorption and the like so as to obtain isopropyl alcohol for a liquid chromatography-mass spectrometer. By the purification method of isopropyl alcohol for a liquid chromatography-mass spectrometer, isopropyl alcohol 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, isopropyl alcohol obtained after purification can be applied in the field of liquid chromatography-mass spectrometers, and the application range of isopropyl alcohol is broadened.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying isopropanol 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 s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/10C07C29/74
Inventor 范文林张群星张怡陈建辉
Owner 上海星可高纯溶剂有限公司
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