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Purification method of gradient elution solvent acetonitrile

A technology of elution solvent and purification method, applied in the direction of carboxylic acid nitrile purification/separation, organic chemistry, etc., can solve the problems of high degree of containment and high cost, and achieve the effects of simple production process, stable operation and cost reduction.

Inactive Publication Date: 2015-11-25
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

High-purity acetonitrile mostly relies on imports, resulting in higher costs and a greater degree of restraint by foreign technology

Method used

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  • Purification method of gradient elution solvent acetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The purification method of gradient elution solvent acetonitrile is characterized in that, comprises the steps:

[0023] a. get the raw material acetonitrile with a purity of 99.5% (wt), add sodium carbonate and adjust the pH of the solution to 7, and shake to make the organic acid impurities in the sodium carbonate and the raw material acetonitrile fully react to generate salt precipitates; Separate the layers, discard the aqueous layer, filter the organic layer, and keep the filtrate.

[0024] Pass the above-mentioned filtrate into the adsorbent column equipped with 3A molecular sieve with aluminum hydroxide attached on the surface at a rate of 20 column volumes / hour, further remove the moisture in the organic layer, and remove aromatic hydrocarbons and polar compounds in acetonitrile at the same time Impurities. The mass concentration of aluminum hydroxide is 0.5%, and the particle size of 3A molecular sieve is 100 mesh. After adsorption, the water content of the a...

Embodiment 2

[0029] The purification method of gradient elution solvent acetonitrile is characterized in that, comprises the steps:

[0030] a. get the raw material acetonitrile with purity of 99.5% (wt), add sodium carbonate and adjust the pH of the solution to 8, and shake to make sodium carbonate fully react with the organic acid impurities in the raw material acetonitrile to generate salt precipitate; Separate layers, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0031] Pass the above-mentioned filtrate into the adsorbent column equipped with 3A molecular sieve with aluminum hydroxide attached on the surface at a rate of 30 column volumes / hour, to further remove the moisture in the organic layer, and at the same time remove the aromatic hydrocarbons and polar compounds in acetonitrile Impurities. The concentration of aluminum hydroxide is 1.5%, and the particle size of 3A molecular sieve is 20 mesh. After adsorption, the water content o...

Embodiment 3

[0036] The purification method of gradient elution solvent acetonitrile is characterized in that, comprises the steps:

[0037] a. get the raw material acetonitrile with purity of 99.5% (wt), add sodium carbonate and adjust the pH of solution to 7.5, and shake to make sodium carbonate fully react with the organic acid impurities in the raw material acetonitrile to generate salt precipitate; Separate layers, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0038]Pass the above filtrate into the adsorbent column equipped with 4A molecular sieve with aluminum hydroxide attached on the surface at a rate of 0.5 column volume / hour, further remove the moisture in the organic layer, and remove aromatic hydrocarbons and polar compounds in acetonitrile at the same time Impurities. The concentration of aluminum hydroxide is 0.9%, and the particle size of 4A molecular sieve is 60 mesh. After adsorption, the water content of acetonitrile is co...

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Abstract

The invention discloses a purification method of a gradient elution solvent acetonitrile. The method is characterized in that impurities in a raw material acetonitrile are removed through processes such as modified active carbon, ion exchange resin adsorption and the like so as to obtain the gradient elution solvent acetonitrile with its purity being greater than or equal to 99.99 wt%. By the purification method of the gradient elution solvent acetonitrile, a gradient elution solvent acetonitrile which can be applied in the field of gradient elution can be obtained.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying gradient elution solvent acetonitrile. Background technique [0002] Gradient elution is also called gradient elution or program elution. In gas chromatography, in order to improve the separation of samples with a wide boiling range and shorten the analysis period, the method of temperature programming is widely used. In liquid chromatography, gradient elution is used for samples with complex components. That is, in the same analysis cycle, the concentration ratio of the mobile phase is continuously changed according to a certain procedure, which is called gradient elution. Therefore, components with large property differences in a complex sample can be separated according to their appropriate capacity factor k. [0003] The mobile phase is composed of several elution solvents with different polarities, and the polarity of the mobile phase is changed ...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/34
Inventor 范文林张群星张怡潘祖义
Owner 上海星可高纯溶剂有限公司
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