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Purification method of chromatographic grade methanol

A purification method and chromatographic-level technology, which is applied in the field of solvent purification, can solve the problems of high-purity methanol dependence on imports, high degree of containment, and low methanol output, and achieve stable operation, simple production process, and high yield.

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

[0003] There are few reports on the preparation methods of methanol liquid chromatography reagents in my country, and the domestic methanol production is relatively low, and the purity is not high.

Method used

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  • Purification method of chromatographic grade methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0021] a. get the raw material methyl alcohol that purity is 99.5% (wt), add sodium carbonate to make the solution p Adjust the H to 7, and shake to make the sodium carbonate fully react with the acidic impurities in the raw material methanol to form a salt precipitate; stand for stratification, discard the water layer and the 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 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, the methanol water content is controlled at≤0.03%; In the step, the molecular sieve is used to remove the moisture in the methanol after extraction. If the moisture content is >0.03%, the molecular sieve needs to be replaced before continuing t...

Embodiment 2

[0029] The purification method of chromatographic grade methanol comprises the steps:

[0030] a. get the raw material methyl alcohol that purity is 99.5% (wt), add Potassium Hydroxide and adjust the pH of solution to 8, and shake and make Potassium Hydroxide and the acidic impurity in the raw material methanol fully react, generate salt precipitate; Static Separate the layers, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0031] b. Adsorption:

[0032] 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, the methanol water content is controlled at≤0.03%; In the step, the molecular sieve is used to remove the moisture in the methanol after extraction. If the moisture content is >0.03%, the molecular sieve needs to be replaced before continuing the mol...

Embodiment 3

[0038] The purification method of chromatographic grade methanol comprises the steps:

[0039] a. get the raw material methyl alcohol that purity is 99.5% (wt), add sodium oxide and adjust the pH of solution to 7.5, and shake to make the acidic impurities in sodium oxide and raw material methanol fully react, generate salt precipitate; layer, discard the aqueous layer and precipitate, filter the organic layer, and keep the filtrate.

[0040] b. Adsorption:

[0041] 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 methanol water content is controlled at≤0.03%; this step Use molecular sieve to remove the moisture in methanol after extraction, if the moisture content > 0.03%, you need to replace the molecular sieve and then continue the molecular sieve adsorption treatment;

[0042] II. ...

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Abstract

The invention discloses a method for purifying chromatographic-grade methanol, which is characterized in that impurities in raw methanol are removed through processes such as modified activated carbon adsorption to obtain chromatographic-grade methanol. The method for purifying chromatographic grade methanol provided by the present invention can obtain methanol with a purity ≥ 99.99% (wt), which meets the high purity requirements of chromatographic grade reagents, and enables the purified methanol to be applied to fields such as chromatographic analysis, chromatographic separation, and chromatographic preparation. , expanding the scope of application.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying chromatographic grade methanol. 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, methanol 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 met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/04C07C29/76
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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