CN102060674A - Method for purifying high-purity organic solvent diethyl ether - Google Patents
Method for purifying high-purity organic solvent diethyl ether Download PDFInfo
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- CN102060674A CN102060674A CN2010106118418A CN201010611841A CN102060674A CN 102060674 A CN102060674 A CN 102060674A CN 2010106118418 A CN2010106118418 A CN 2010106118418A CN 201010611841 A CN201010611841 A CN 201010611841A CN 102060674 A CN102060674 A CN 102060674A
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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
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 ether.
Background technology
The ether reagent content of Xiao Shouing is about 99.5% on the market, wherein contains 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 every technical indicator 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 ether, this purification process have characteristics such as technology is simple, impurity is easily separated, product purity height.
The present invention is by following scheme implementation:
A kind of purification process of high-purity organic solvent 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, and the ether fluid temperature is 40 ℃～45 ℃ in the still, 34 ℃～35 ℃ of still top temperature, control reflux ratio 1: 0.5～3, the rectifying after-filtration promptly obtains chromatographic grade ether product.
And described sorbent material is an activated alumina, and siccative is a Calcium Chloride Powder Anhydrous.
And, described raw material ether with the 40-80mL/min velocity flow through the activated alumina adsorption column.
And described siccative is a Calcium Chloride Powder Anhydrous.
Advantage of the present invention and positively effect are:
1, the present invention is that 99.5% ether is raw material, carries out fractionation by adsorption with activated alumina as sorbent material and remove wherein impurity with content; 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; the product purity height; 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 remarkable economic efficiency.
3, the product of this purification process production after testing its every index 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 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 interior dress 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, impurity such as superoxide are adsorbed, detect absorption fluid quality, it (is that the every index of effluent liquid is near chromatographic grade technical requirement that fluid to be adsorbed 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) the effusive ether of above-mentioned adsorption column is entered dry post, the high 1.6M of post, diameter 4.2cm packs into through baking exsiccant 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, illustrates siccative greater than 0.1% o'clock by water saturation, carry out drying treatment after must changing again.
(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 fluid 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 promptly 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 interior dress 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, and diameter 4.2cm packs into through baking exsiccant Calcium Chloride Powder Anhydrous, measures the water content of dry back ether, and 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 drying treatment after must changing again.
(3) the stainless steel rectifying still that above-mentioned ether is after drying 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 fluid 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 promptly 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 (4)
1. the purification process of a high-purity organic solvent ether, it is characterized in that: 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, and the ether fluid temperature is 40 ℃～45 ℃ in the still, 34 ℃～35 ℃ of still top temperature, control reflux ratio 1: 0.5～3, the rectifying after-filtration promptly obtains chromatographic grade ether product.
2. the purification process of a kind of high-purity organic solvent ether according to claim 1 is characterized in that: described sorbent material is an activated alumina, and siccative is a Calcium Chloride Powder Anhydrous.
3. the purification process of a kind of high-purity organic solvent ether according to claim 1 is characterized in that: described raw material ether with the 40-80mL/min velocity flow through the activated alumina adsorption column.
4. the purification process of a kind of high-purity organic solvent ether according to claim 1 is characterized in that: described siccative is a Calcium Chloride Powder Anhydrous.
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| CN 201010611841 CN102060674B (en) | 2010-12-29 | 2010-12-29 | Method for purifying high-purity organic solvent diethyl ether |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN102531818A (en) * | 2011-12-26 | 2012-07-04 | 天津市康科德科技有限公司 | Preparation method of 30-60 DEG C petroleum ether of chromatographic grade organic solvent |
| CN102584543A (en) * | 2011-12-26 | 2012-07-18 | 天津市康科德科技有限公司 | Preparation method of chromatographic-grade organic solvent ethylene glycol monomethyl ether |
| CN107501056A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatogram absolute ether and preparation method thereof, production system |
| CN111153778A (en) * | 2018-11-08 | 2020-05-15 | 杭州纤纳光电科技有限公司 | Method for purifying diethyl ether and method for improving purity of nitrogen-containing organic matter by using diethyl ether |
Citations (3)
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|---|---|---|---|---|
| US2485329A (en) * | 1946-04-05 | 1949-10-18 | Standard Oil Dev Co | Ether purification |
| US3847756A (en) * | 1972-11-09 | 1974-11-12 | Eastman Kodak Co | Recovery of diethyl ether from an olefin hydration product stream by extractive distillation with water |
| JPS5473711A (en) * | 1977-11-16 | 1979-06-13 | Nippon Gousei Arukooru Kk | Purification of ethyl ether |
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2010
- 2010-12-29 CN CN 201010611841 patent/CN102060674B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2485329A (en) * | 1946-04-05 | 1949-10-18 | Standard Oil Dev Co | Ether purification |
| US3847756A (en) * | 1972-11-09 | 1974-11-12 | Eastman Kodak Co | Recovery of diethyl ether from an olefin hydration product stream by extractive distillation with water |
| JPS5473711A (en) * | 1977-11-16 | 1979-06-13 | Nippon Gousei Arukooru Kk | Purification of ethyl ether |
Non-Patent Citations (2)
| Title |
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| 吴庆华: "回收纯化乙醚新方法研究", 《粮油仓储科技通讯》 * |
| 李桂英: "提纯、分离乙醚方法改进", 《张家口师专学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN102531818A (en) * | 2011-12-26 | 2012-07-04 | 天津市康科德科技有限公司 | Preparation method of 30-60 DEG C petroleum ether of chromatographic grade organic solvent |
| CN102584543A (en) * | 2011-12-26 | 2012-07-18 | 天津市康科德科技有限公司 | Preparation method of chromatographic-grade organic solvent ethylene glycol monomethyl ether |
| CN107501056A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatogram absolute ether and preparation method thereof, production system |
| CN111153778A (en) * | 2018-11-08 | 2020-05-15 | 杭州纤纳光电科技有限公司 | Method for purifying diethyl ether and method for improving purity of nitrogen-containing organic matter by using diethyl ether |
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| CN102060674B (en) | 2013-05-29 |
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