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Purification method of chromatographic grade tetrahydrofuran

A technology of tetrahydrofuran and a purification method, which is applied in the field of purification of chromatographic grade tetrahydrofuran, can solve the problems of large degree of restraint and high cost, and achieve the effects of simple production process, stable operation and low energy consumption

Active Publication Date: 2018-03-06
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 tetrahydrofuran 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 tetrahydrofuran

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Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0021] a. take the raw material tetrahydrofuran with a purity of 99.5 wt%, add sodium carbonate to adjust the pH of the solution to 7, and shake to make the sodium carbonate fully react with the acidic impurities in the raw material tetrahydrofuran to generate salt precipitates; stand for stratification, Discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0022] b. Adsorption:

[0023] 1. The above-mentioned filtrate is passed into the adsorbent column that the 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 the adsorption, the tetrahydrofuran water content is controlled at≤0.03%; In the step, the molecular sieve is used to remove the moisture in the extracted tetrahydrofuran. If the moisture content is >0.03%, the molecular sieve needs to be...

Embodiment 2

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

[0029] a. get the raw material tetrahydrofuran with a purity of 99.5wt%, add potassium hydroxide to adjust the pH of the solution to 8, and shake to make the acidic impurities in the potassium hydroxide and the raw material tetrahydrofuran fully react to generate salt precipitates; layer, 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 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, THF water content is controlled at≤0.03%; In the step, the molecular sieve is used to remove the moisture in the extracted tetrahydrofuran. If the moisture content is >0.03%, the molecular sieve needs to be replaced before continuing the molecula...

Embodiment 3

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

[0037] a. Take the raw material tetrahydrofuran 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 tetrahydrofuran to generate salt precipitates; stand for stratification, 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 tetrahydrofuran water content is controlled at≤0.03%; this step Use molecular sieve to remove the moisture in THF after extraction, if the moisture content > 0.03%, you need to replace the molecular sieve and then continue the ...

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Abstract

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

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying chromatographic grade tetrahydrofuran. 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 an excellent liquid chromatographic reagent, tetrahydrofuran has the characteristics of fast dissolution rate and good permeation and diffusion performance. Quantitative analysis etc. [0003] There are few reports on the preparation methods of tetrahydrofura...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08
CPCC07D307/08
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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