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Purification method of chromatographic grade n-propanol

A purification method and technology for n-propanol, which are applied in chemical instruments and methods, separation/purification of hydroxyl compounds, preparation of organic compounds, etc. The production process is simple, the operation is stable, and the yield is high.

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

The yield of n-propanol prepared by the above method is low, and also contains impurities such as aldehydes, olefins, allyl alcohol and water, and the purity is not high
High-purity n-propanol 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 n-propanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The purification method of chromatographic grade n-propanol comprises the steps:

[0021] a. get the raw material n-propanol with a purity of 99.5% (wt), add sodium carbonate to adjust the pH of the solution to 7, and shake to make the acidic impurities in the sodium carbonate and the raw material n-propanol fully react to generate salt precipitates ; Static layering, discard the water layer and precipitate, filter the organic layer, retain the filtrate.

[0022] b. Adsorption:

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

Embodiment 2

[0028] The purification method of chromatographic grade n-propanol comprises the steps:

[0029] a. get raw material n-propanol with a purity of 99.5% (wt), add potassium hydroxide to adjust the pH of the solution to 8, and shake to make potassium hydroxide fully react with the acidic impurities in the raw material n-propanol to generate salts Precipitate; leave to separate layers, discard the water 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 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 adsorption, n-propanol water content is controlled at≤0.03% In this step, molecular sieves are used to remove the moisture in the extracted n-propanol. If the moisture content is > 0.03%, the molecular sieve needs to be replaced before continuing the molecular...

Embodiment 3

[0036] The purification method of chromatographic grade n-propanol comprises the steps:

[0037] a. get the raw material n-propanol with a purity of 99.5% (wt), add sodium oxide to adjust the pH of the solution to 7.5, and shake to make the sodium oxide fully react with the acidic impurities in the raw material n-propanol to generate salt precipitates ; Static layering, discard the water layer and precipitate, filter the organic layer, retain the filtrate.

[0038] b. Adsorption:

[0039] 1. above-mentioned filtrate is passed into the adsorbent column that particle diameter is 100 mesh molecular sieves with the speed of 15 column volumes / hour, further removes the moisture in the organic layer; After adsorption, n-propanol water content is controlled at≤0.03%; In this step, the molecular sieve is used to remove the moisture in the extracted n-propanol. If the moisture content is >0.03%, the molecular sieve needs to be replaced before continuing the molecular sieve adsorption t...

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Abstract

The invention discloses a purification method of chromatographic grade n-propanol. The method is characterized in that impurities in a raw material n-propanol are removed through processes such as modified active carbon adsorption and the like so as to obtain the chromatographic grade n-propanol. By the purification method of the chromatographic grade n-propanol, n-propanol 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, n-propanol obtained after purification can be applied in fields of chromatographic analysis, chromatographic separation, chromatographic preparation and the like, and the application range of n-propanol is broadened.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying chromatographic grade n-propanol. 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, n-propanol is used for liquid chromatography analysis and is widely used in the fields of medicine, chemical industry, inspection analysis, and detection. N-propanol can also be used as a solvent for vegetable oils,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/76C07C29/88C07C31/10
Inventor 范文林张群辉王洪纪王洋
Owner 上海星可高纯溶剂有限公司
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