CN102381946A - Preparation method of ether eluent - Google Patents

Abstract

The invention relates to a preparation method of an ether eluent, which comprises the following steps of: removing peroxide in ether with a sodium bisulfite solution or ferrous sulfate solution, drying with anhydrous calcium chloride, filtrating and distilling, placing the distilled ether in a dying bottle, drying the ether with sodium metal, and storing under ventilation for 24 hour; and placing the ether in a reaction kettle with a 1.5 m distillation column and adding a small amount of sodium metal wire strip for distillation to obtain the high-purity chromatographic-grade anhydrous ether. The anhydrous ether prepared by the method provided by the invention has high purity, and the peroxide, water, ethanol and other impurities are effectively removed, thus the anhydrous ether can reach the standard of a chromatographic-grade reagent.

Description

The preparation method of ether eluent

Technical field

The invention belongs to the preparation field of organic solvent, relate in particular to a kind of preparation method of ether eluent.

Background technology

Ether (C ₂H ₅OC ₂H ₅Mol74.12) be a kind of organic solvent commonly used, purposes extremely widely arranged at organic synthesis, chemical analysis, scientific research and education, industrial production and pharmaceutical sanitary field.In the last few years since various countries to narcotic use attention especially.

In the industry ether, often contain aldehyde, water, ethanol and superoxide, also contain trace acetone sometimes.If it is improper to store, also possibly produce superoxide.The existence of these impurity, experiment and production that ask for something is made solvent with anhydrous diethyl ether are inappropriate, when particularly having superoxide to exist, the danger that also can blast.The anhydrous diethyl ether free from foreign meter and that purity is higher of purifying out seems particularly important.

Summary of the invention

The preparation method who the purpose of this invention is to provide a kind of ether eluent.

The technical scheme that realizes the object of the invention is following:

A kind of preparation method of ether eluent, step is following:

(1) gets 500 milliliters common ether, add sodium sulfite solution or 10 milliliters of copperas solutions of 50 milliliter 10%, add 100 ml water shake wells again, tell the ether layer, use the saturated common salt solution washed twice, use Calcium Chloride Powder Anhydrous dry again;

(2) will filter through the dried ether of step (1), distillation with the ether that steams, is placed in the drying bottle, and is dry with sodium Metal 99.5, and ventilation is preserved, and places 24 hours;

(3) will put into the reaction kettle that 1.5 meters rectifying volumns are housed and add the rectifying of sodium Metal 99.5 strand through the dried anhydrous diethyl ether of step (2), get middle runnings, obtain high purity chromatographic grade anhydrous diethyl ether.

Advantage of the present invention and beneficial effect are:

The anhydrous diethyl ether of the inventive method preparation, purity is high, effectively must remove impurity such as superoxide, water, ethanol, can reach the standard of chromatographic grade reagent.

Embodiment

Below in conjunction with specific embodiments the present invention is further specified,, can not limit protection scope of the present invention with following illustrating to help understanding content of the present invention.

Embodiment 1:

A kind of preparation method of ether eluent, step is following:

(1) gets 500 milliliters common ether, place in 1000 milliliters the separating funnel, add 50 milliliter 10% freshly prepared sodium sulfite solution; Or add 10 milliliters of copperas solutions and 100 ml water shake wells or the ether layer is told in stirring (then can not omit this step if do not contain superoxide in the ether) then, use the saturated common salt solution washed twice, with the Calcium Chloride Powder Anhydrous drying.

(2) will filter distillation through dried ether.With the ether that steams, be placed in the exsiccant bottle, dry with sodium Metal 99.5.If ether is dry not enough, can produce great amount of bubbles.Ventilation is preserved, and places 24 hours

(3) dried anhydrous diethyl ether is put into the reaction kettle of the rectifying volumn that is equipped with 1.5 meters and add the rectifying of little metal sodium strand.Get middle runnings, can obtain high purity chromatographic grade anhydrous diethyl ether

The preparation of copperas solution: get 100 ml waters, slowly add 6 milliliters of vitriol oils, add 60 gram ferrous sulfate dissolvings again and get final product.Therefore the easy deterioration by oxidation of copperas solution postpone of a specified duration needs before use preparation temporarily.When using purer ether to produce anhydrous diethyl ether, can remove the copperas solution washing from.

For preventing that ether storage from producing superoxide in storing, except that avoid as far as possible with light with air contacts, can in ether, add a little iron filings, copper scale or exsiccant Pottasium Hydroxide.

Discuss

(1) because the existence of still substrate sodium, the evaporate to dryness of trying not during distillation.

(2) distill moisture Ex-all basically for the first time, safety assurance is provided for sodium Metal 99.5 uses.

(3) storage temperature must not be higher than room temperature.

(4) operating process should be ventilated, and avoids naked light.

Claims (1)

1. the preparation method of an ether eluent, it is characterized in that: step is following:

(1) gets 500 milliliters ether, add sodium sulfite solution or 10 milliliters of copperas solutions of 50 milliliter 10%, add 100 ml water shake wells again, tell the ether layer, use the saturated common salt solution washed twice, use Calcium Chloride Powder Anhydrous dry again;

(2) will filter through the dried ether of step (1), distillation with the ether that steams, is placed in the drying bottle, and is dry with sodium Metal 99.5, and ventilation is preserved, and places 24 hours;

(3) will put into the reaction kettle that 1.5 meters rectifying volumns are housed and add the rectifying of sodium Metal 99.5 strand through the dried anhydrous diethyl ether of step (2), obtain high purity chromatographic grade anhydrous diethyl ether.