CN102060674B

CN102060674B - Method for purifying high-purity organic solvent diethyl ether

Info

Publication number: CN102060674B
Application number: CN 201010611841
Authority: CN
Inventors: 宋金链; 张玉芝
Original assignee: Tianjin Concord Technology Co Ltd
Current assignee: Tianjin Concord Technology Co Ltd
Priority date: 2010-12-29
Filing date: 2010-12-29
Publication date: 2013-05-29
Anticipated expiration: 2030-12-29
Also published as: CN102060674A

Abstract

The invention relates to a method for purifying high-purity organic solvent diethyl ether, comprising the steps of: adsorbing diethyl ether as a raw material with activated aluminium oxide to remove impurities of peroxide and the like, drying with a drying agent for dewatering, rectifying with a rectifying kettle, filtering and sealing to obtain a diethyl ether product of a high performance liquid chromatography (HPLC) level. By means of the method, a chromatographic diethyl ether product with the purity more than 99.9% can be obtained, the yield is more than 94%, and the qualification rate is more than 94%, so that the requirement on users of the HPLC reagent diethyl ether in the aspects of scientific experiments, subject study and the like is met; meanwhile, compared with a conventional method, the method provided by the invention has the advantages of high product purity, simplicity and convenience of operation and stable product quality, and is suitable for scale production.

Description

A kind of purification process of high-purity organic solvent diethyl ether

Technical field

The invention belongs to chemical technology field, relate to the purification process of organic solvent, especially a kind of purification process of high-purity organic solvent diethyl ether.

Background technology

The ether reagent content of selling on the market is about 99.5%, wherein contains the impurity such as a small amount of carbonyl, pure and mild superoxide and water.This kind ether can not satisfy the needs of related science research trial, so this kind ether must be through being further purified, and making its all technical all reach chromatographic grade standard could use.

At present, domestic data about ether purifying aspect mainly is because few through the content of impurity in the ether of preliminary purification seldom, is difficult in the rectifying impurity is removed, and therefore, the present invention be directed to this technical barrier and proposes effective solution.

Summary of the invention

The purification process that the purpose of this invention is to provide a kind of high-purity organic solvent diethyl ether, this purification process have that technique is simple, impurity is easily separated, the product purity high.

The present invention is by following scheme implementation:

A kind of purification process of high-purity organic solvent diethyl ether, the step of purifying is as follows:

(1) the raw material ether is adsorbed by the adsorption column that sorbent material is housed;

(2) ether after will adsorbing carries out drying with siccative, and measures water content, ether water content≤0.03%;

(3) water content after the drying is carried out rectifying at the ether of acceptability limit, the condition of rectifying is: temperature is 80～100 ℃ at the bottom of the rectifying still, the ether solution temperature is 40 ℃～45 ℃ in the still, 34 ℃～35 ℃ of still top temperature, control reflux ratio 1: 0.5～3, filter after the rectifying, namely obtain chromatographic grade ether product.

And described sorbent material is activated alumina, and siccative is Calcium Chloride Powder Anhydrous.

And described raw material ether is with the 40-80mL/min speed activated alumina adsorption column of flowing through.

And described siccative is Calcium Chloride Powder Anhydrous.

Advantage of the present invention and positively effect are:

1, the present invention take the ether of content as 99.5% as raw material, carry out fractionation by adsorption with activated alumina as sorbent material and remove wherein impurity; adopt Calcium Chloride Powder Anhydrous to remove wherein moisture as siccative; obtain the ether product of purity 99.9% through absorption, drying, rectifying purifying; this purification process is simple; product purity is high; stable, be suitable for large-scale production.

2, this purification process promotes ether content to 99.9%, and all other chromatogram indexs all reach requirement, and yield rate is increased to more than 90% by original 75%, saved manpower, reduce the consumption of the energy, more be applicable to industrialized production and application, had significant economic benefit.

3, the product of this purification process production after testing its indices meet the requirement of chromatographically pure ether, its ether content is greater than 99.9%, the rate of recovery is greater than 94%, yield rate reaches 94%, and this product can satisfy the application demand of user aspect scientific experiment, subject study of high performance liquid chromatography (HPLC).

Specific embodiment

The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.

Embodiment 1:

A kind of purification process of high-purity organic solvent diethyl ether, step is as follows:

(1) raw material ether (content is about 99.5%) is promoted to adsorption column top, the high 1.6M of adsorption column wherein, diameter 4.2cm, the amount of in-built activated alumina adsorbents be post high 4/5, the ether raw material adsorbs with 40mL/min speed;

In post, ether fully contacts with activated alumina adsorbents, the impurity such as superoxide are adsorbed, detect absorption fluid quality, it (is that the effluent liquid indices is near chromatographic grade technical requirement that fluid upon adsorption is up to the standards, its concrete technical requirement sees Table 1) after enter next-step operation, and remove the high absorption front-end volatiles of impurity.

(2) ether that above-mentioned adsorption column is flowed out enters dry post, the high 1.6M of post, and diameter 4.2cm packs into through toasting dry Calcium Chloride Powder Anhydrous, detects dried ether water content, and moisture controlled is≤0.03%,

Enter next-step operation after water content is qualified; If moisture content greater than 0.1% the time, illustrates siccative by water saturation, carry out again drying treatment after must changing.

(3) the stainless steel rectifying still that above-mentioned ether is after drying flow to into 100L carries out rectifying; utilize heat-conducting oil heating; temperature is about 80 ℃ at the bottom of the control stainless steel still; the ether solution temperature is about 40 ℃ in the still, goes out about 34.6 ℃ of liquid temp, and the control reflux ratio was 1: 0.5 fluid; finished product is behind 0.45 μ m filtering with microporous membrane; the bottling sealing namely obtains chromatographic grade ether product (purity 99.9%) under nitrogen protection, and its front-end volatiles are for further processing.

Embodiment 2:

A kind of purification process of high-purity organic solvent ether, step is as follows:

(1) raw material ether (content is about 99.5%) is promoted to the adsorption column top, the high 1.6M of adsorption column, diameter 4.2cm, the amount of in-built activated alumina adsorbents be post high 4/5, the ether raw material adsorbs with 80mL/min speed, and the absorption fluid enters next-step operation after the assay was approved; And the absorption front-end volatiles that impurity is high are removed;

(2) effluent liquid with above-mentioned adsorption column enters dry post, tower height 1.6M, diameter 4.2cm packs into through toasting dry Calcium Chloride Powder Anhydrous, measure dry after the water content of ether, moisture controlled is≤0.03%,

Enter next-step operation after water content is qualified; When moisture content greater than 0.1% the time, siccative is described by water saturation, carry out again drying treatment after must changing.

(3) the stainless steel rectifying still that above-mentioned after drying ether is flow to into 120L carries out rectifying.Utilize heat-conducting oil heating, temperature is 100 ℃ at the bottom of the control stainless steel still, the ether solution temperature is about 45 ℃ in the still, go out about 35 ℃ of liquid temp, the control reflux ratio was 1: 3 fluid, finished product is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing namely obtains qualified chromatographic grade ether product (purity 99.9%) under nitrogen protection; Its front-end volatiles are for further processing.

Effect detection:

Organic solvent ether after the purification, (the quartzy cuvette of 1cm in ultraviolet wavelength 220nm～400nm scope, water is made reference), absorbancy satisfies the index request in the table 1, content is greater than 99.9%, moisture≤0.03%, and the rate of recovery is greater than 94%, yield rate reaches more than 94% approximately, and all other indexs are the value of touching the mark all.

Table 1: the technical indicator of raw material, chromatographic grade ether

Claims

1. the purification process of a high-purity organic solvent diethyl ether, it is characterized in that: the step of purifying is as follows:

⑴ adsorb the raw material ether by the adsorption column that sorbent material is housed; Described raw material ether is the ether of content 99.5%;

⑵ the ether after will adsorb carries out drying with siccative, and measures water content, ether water content≤0.03%;

With drying after water content carry out rectifying at the ether of acceptability limit, the condition of rectifying is: temperature is 80 ~ 100 ℃ at the bottom of the rectifying still, the ether solution temperature is 40 ℃ ~ 45 ℃ in the still, 34 ℃ ~ 35 ℃ of still top temperature, filter after the rectifying control reflux ratio 1:0.5 ~ 3, namely obtains chromatographic grade ether product;

Described sorbent material is activated alumina, and siccative is Calcium Chloride Powder Anhydrous.

2. the purification process of a kind of high-purity organic solvent diethyl ether according to claim 1 is characterized in that: described raw material ether is with the 40-80mL/min speed activated alumina adsorption column of flowing through.