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Purification method of chromatographic grade ethanol

A purification method and a chromatographic-grade technology, which are applied in the field of solvent purification, can solve the problems of low ethanol yield, high degree of containment and low purity, and achieve the effects of simple production process, stable operation and high yield.

Active 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

[0003] There are few reports on the preparation methods of ethanol liquid chromatography reagents in my country, and the domestic ethanol production is low, containing impurities such as aldehydes, benzenes, water, etc., and the purity is not high
High-purity ethanol 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 chromatographic grade ethanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The purification method of chromatographic grade ethanol comprises the steps:

[0021] a. get the raw material ethanol that purity is 99.5% (wt), add sodium carbonate and adjust the pH of solution to 7, and shake to make the acidic impurities in sodium carbonate and raw material ethanol fully react, generate salt precipitate; layer, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0022] b. Adsorption:

[0023] 1. above-mentioned filtrate is passed into the adsorbent column that particle diameter is 50 purpose 3A molecular sieves with the speed of 0.5 column volume / hour, further removes the moisture in the organic layer; After adsorption, ethanol water content is controlled at≤0.03%; In the step, molecular sieves are used to remove the moisture in the extracted ethanol. If the moisture content is >0.03%, the molecular sieves need to be replaced before continuing the molecular sieve adsorption treatment;

[0024] II. Then, t...

Embodiment 2

[0028] The purification method of chromatographic grade ethanol comprises the steps:

[0029] a. get the raw material ethanol that purity is 99.5% (wt), add potassium hydroxide and adjust the pH of solution to 8, and shake to make potassium hydroxide fully react with the acidic impurities in the raw material ethanol, generate salt precipitate; Static Separate the layers, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0030] b. Adsorption:

[0031] 1. the above-mentioned filtrate is passed into the adsorbent column that the particle diameter is 20 order 3A molecular sieves with the speed of 30 column volumes / hour, further removes the moisture in the organic layer; after the adsorption, the ethanol water content is controlled at≤0.03%; In the step, molecular sieves are used to remove the moisture in the extracted ethanol. If the moisture content is >0.03%, the molecular sieves need to be replaced before continuing the molecular sie...

Embodiment 3

[0036] The purification method of chromatographic grade ethanol comprises the steps:

[0037] a. get the raw material ethanol whose purity is 99.5% (wt), add sodium oxide and adjust the pH of the solution to 7.5, and shake to make the acidic impurities in the sodium oxide and the raw material ethanol fully react to generate salt precipitate; layer, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0038] b. Adsorption:

[0039] 1. the above-mentioned filtrate is passed into the adsorbent column that the particle size is 100 mesh molecular sieves with the speed of 15 column volumes / hour, and further removes the moisture in the organic layer; after the adsorption, the ethanol water content is controlled at≤0.03%; this step Use molecular sieve to remove the moisture in the extracted ethanol, if the moisture content > 0.03%, you need to replace the molecular sieve and then continue the molecular sieve adsorption treatment;

[0040] II....

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Abstract

The invention discloses a purification method of chromatographic grade ethanol. The method is characterized in that impurities in a raw material ethanol are removed through processes such as modified active carbon adsorption and the like so as to obtain the chromatographic grade ethanol. By the purification method of chromatographic grade ethanol, ethanol with its purity being greater than or equal to 99.99 wt% can be obtained. The method meets high-purity requirement of a chromatographic grade reagent. Therefore, ethanol obtained after purification can be applied in fields of chromatographic analysis, chromatographic separation, chromatographic preparation and the like, and the application range of ethanol is broadened.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying chromatographic grade ethanol. Background technique [0002] Chromatographic reagents refer to chemical reagents used for chromatographic analysis, chromatographic separation, and chromatographic preparation. Because there are many types of chromatography and the process is complicated, the chromatographic reagents are classified into various chromatographic reagents, such as: gas chromatography reagents, high pressure liquid chromatography reagents, thin layer chromatography reagents, column chromatography reagents, ion chromatography reagents, ion pairs Chromatographic reagents, etc. As a high-performance liquid chromatography reagent, ethanol is used for liquid chromatography analysis and is widely used in the fields of medicine, chemical industry, inspection analysis, and detection. [0003] There are few reports on the preparation methods of ethan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/08C07C29/76
Inventor 范文林张群星王洪纪王洋
Owner 上海星可高纯溶剂有限公司
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