CN102040455A - Purification method of chromatographically pure organic solvent cyclohexane - Google Patents
Purification method of chromatographically pure organic solvent cyclohexane Download PDFInfo
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- CN102040455A CN102040455A CN2010106118422A CN201010611842A CN102040455A CN 102040455 A CN102040455 A CN 102040455A CN 2010106118422 A CN2010106118422 A CN 2010106118422A CN 201010611842 A CN201010611842 A CN 201010611842A CN 102040455 A CN102040455 A CN 102040455A
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Abstract
The invention relates to a purification method of chromatographically pure organic solvent cyclohexane. The method mainly comprises the following steps of: adsorbing and separating by using an adsorbent, namely silica gel to remove trace benzene and impurities with high ultraviolet absorption, drying by using calcium hydride to remove moisture from the cyclohexane, and rectifying and purifying, and removing the trace impurities from the cyclohexane step by step. By the method, the chromatograph cyclohexane product with purity of more than or equal to 99.9 percent can be obtained, the yield is more than or equal to 95 percent, and the purified reagent meets the high performance liquid chromatography (HPLC) reagent cyclohexane requirement of a customer.
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 chromatographically pure organic solvent hexanaphthene.
Background technology
Hexanaphthene is one of industrial widely used non-polar hydrocarbon kind solvent.Hexanaphthene is to make with purified petroleum benzin hydrogenation in the presence of catalyst, wherein contains the high impurity of micro-benzene class, uv-absorbing and water etc.For removing trace impurity, we have carried out a large amount of experiments, have chosen absorption, exsiccant purification process, and it is complicated to have replaced technological process, and quality product can not reach the common process of scientific research requirement.
The domestic method that is further purified about high purity hexanaphthene reagent is set forth very few, mainly be because very few through the content of impurity in the hexanaphthene of preliminary purification, be difficult to small amount of impurities is removed in the general rectifying, therefore, The present invention be directed to this technical barrier and propose effective solution.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of purification process that utilizes the removal of impurities of sorbent material silica gel, uses the dry hexanaphthene of hydrolith is provided, this method has the product purity height, and is easy and simple to handle, stable, is suitable for characteristics such as suitability for industrialized production.
The present invention realizes that the technical scheme of purpose is:
A kind of purification process of chromatographically pure organic solvent hexanaphthene is characterized in that: the step of purifying is as follows:
(1) the raw material hexanaphthene is adsorbed by the adsorption tower that sorbent material is housed;
(2) hexanaphthene after will adsorbing carries out drying with siccative, measures water content, and water content is controlled at≤and 0.02%;
(3) water content after the drying is qualified hexanaphthene carries out rectifying, the condition of rectifying is: at the bottom of the rectifying still in 150 ℃～200 ℃ of temperature, the still hexanaphthene fluid temperature be 85 ℃, rectifying goes out 80 ℃～81 ℃ of liquid temps, control reflux ratio 10: 4～8, the rectifying after-filtration, promptly obtains chromatographically pure organic solvent hexanaphthene.
And described sorbent material is a silica gel, and its particle diameter is 0.15mm～0.25mm, and siccative is a hydrolith.
And, described raw material hexanaphthene with the 50-100mL/min velocity flow through the sorbent material tower, with 30-50mL/min velocity flow drying post.
Advantage of the present invention and positively effect are:
1, the present invention takes the method for rectifying after sorbent material silica gel adsorption, the hydrolith drying progressively to remove wherein trace impurity, and is simple and easy to do, makes the rectifying time save about 4～8 hours, and yield rate brings up to 95% by original 70%～80%.
2, the present invention compares with ordinary method, and this method has the product purity height, and is easy and simple to handle, stable, is suitable for the characteristics of suitability for industrialized production.
3, the present invention can obtain the chromatogram hexanaphthene product of purity 〉=99.9%, and yield 〉=95%, the reagent behind the purifying satisfy the client's of reagents for high performance liquid chromatography (HPLC) hexanaphthene demand.
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 chromatographically pure organic solvent hexanaphthene, its step is as follows:
1, raw material hexanaphthene (content is about 99.5%) is promoted to adsorption tower top, absorption tower height 2.0M, diameter 5.0cm, in pack into the amount of sorbent material silica gel be 4/5 of tower height, the hexanaphthene raw material adsorbs with 50mL/min speed; In tower, hexanaphthene fully contacts with sorbent material silica gel, and micro-benzene and a small amount of high impurity of uv-absorbing are adsorbed, and detects absorption fluid quality, until absorption fluid be up to the standards (be the every index of effluent liquid near chromatographic grade requirement, specific requirement is as shown in table 1); Remove front-end volatiles;
2, qualified absorption effluent liquid is flow to drying tower, control flow velocity 30mL/min, tower height 2.0M, diameter 5.0cm, the hydrolith of packing into contacts the moisture that sponges wherein with hexanaphthene, measure the water content of dry back hexanaphthene, and moisture controlled is≤0.02%; When moisture content 〉=0.05%, change siccative again and continue hexanaphthene is carried out drying treatment;
3, the stainless steel rectifying still that above-mentioned hexanaphthene is after drying flow to 100L carries out rectifying, utilize heat-conducting oil heating, temperature is about 150 ℃ at the bottom of the control stainless steel still, go out about 80～81 ℃ of liquid temp, the debugging reflux ratio is in 10: 4～6 fluids, hexanaphthene finished product after the rectifying is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing is qualified chromatographic grade hexanaphthene product under nitrogen protection; Wherein front-end volatiles are for further processing.
Embodiment 2:
A kind of purification process of chromatographically pure organic solvent hexanaphthene, its step is as follows:
1, raw material hexanaphthene (content is about 95%) is promoted to the adsorption tower top, absorption tower height 2M, diameter 5.0cm, in pack into the amount of sorbent material silica gel be 4/5 of tower height, the hexanaphthene raw material adsorbs with 100mL/min speed, detects absorption fluid quality, is up to the standards until the absorption fluid; Remove front-end volatiles;
2, will adsorb qualified effluent liquid hexanaphthene and flow to drying tower, control flow velocity 50mL/min, this drying tower tower height 2M, diameter 5.0cm, the hydrolith of packing into, the water content of the dry back of measurement hexanaphthene, moisture controlled is≤0.02%; When moisture content 〉=0.05%, change siccative;
3, the stainless steel rectifying still that above-mentioned hexanaphthene is after drying flow to 120L carries out rectifying, utilize heat-conducting oil heating, make that temperature is 200 ℃ at the bottom of the stainless steel still, go out 80～81 ℃ of liquid temps, the control reflux ratio is in 10: 6～8 fluids, hexanaphthene finished product after the rectifying with 0.45 μ m filtering with microporous membrane after, bottling sealing under nitrogen protection is qualified chromatographic grade hexanaphthene product; Wherein front-end volatiles are for further processing.
Effect detection:
The chromatographically pure organic solvent hexanaphthene of the foregoing description preparation, (the quartzy cuvette of 1cm in ultraviolet wavelength 210nm～400nm scope, water is made reference), absorbancy satisfies the index request in the table 1, content is greater than 99.9%, moisture≤0.02%, and the rate of recovery is greater than 95%, yield rate reaches more than 95% approximately, and all other are the value of touching the mark all.
Table 1: the index of chromatographic grade hexanaphthene
Claims (3)
1. the purification process of a chromatographically pure organic solvent hexanaphthene, it is characterized in that: the step of purifying is as follows:
(1) the raw material hexanaphthene is adsorbed by the adsorption tower that sorbent material is housed;
(2) hexanaphthene after will adsorbing carries out drying with siccative, measures water content, and water content is controlled at≤and 0.02%;
(3) water content after the drying is qualified hexanaphthene carries out rectifying, the condition of rectifying is: at the bottom of the rectifying still in 150 ℃～200 ℃ of temperature, the still hexanaphthene fluid temperature be 85 ℃, rectifying goes out 80 ℃～81 ℃ of liquid temps, control reflux ratio 10: 4～8, the rectifying after-filtration, promptly obtains chromatographically pure organic solvent hexanaphthene.
2. the purification process of chromatographically pure organic solvent hexanaphthene according to claim 1 is characterized in that: described sorbent material is a silica gel, and its particle diameter is 0.15mm～0.25mm, and siccative is a hydrolith.
3. the purification process of chromatographically pure organic solvent hexanaphthene according to claim 1 is characterized in that: described raw material hexanaphthene with the 50-100mL/min velocity flow through the sorbent material tower, with 30-50mL/min velocity flow drying post.
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| CN2010106118422A CN102040455A (en) | 2010-12-29 | 2010-12-29 | Purification method of chromatographically pure organic solvent cyclohexane |
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| CN2010106118422A CN102040455A (en) | 2010-12-29 | 2010-12-29 | Purification method of chromatographically pure organic solvent cyclohexane |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531820A (en) * | 2011-12-26 | 2012-07-04 | 天津市康科德科技有限公司 | Purification method of 2,2,4-trimethylpentane organic solvent of chromatographic grade |
| CN102755763A (en) * | 2012-07-18 | 2012-10-31 | 中国石油化工股份有限公司 | Method for purifying solvent for refining caprolactam crystal |
| CN104744196A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Purifying method of high-purity organic solvent n-hexane |
| CN105085137A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-octane |
| CN105085139A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-heptane |
| CN105085149A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent cyclohexane |
| CN107501031A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatographically pure n-hexane and preparation method thereof, production system |
| CN107522588A (en) * | 2017-08-29 | 2017-12-29 | 湖北工程学院 | Chromatographically pure hexamethylene and preparation method thereof, production system |
| CN110713429A (en) * | 2019-10-29 | 2020-01-21 | 天津康科德医药化工有限公司 | Method for purifying chromatographically pure hexane |
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| US4433194A (en) * | 1983-05-06 | 1984-02-21 | Uop Inc. | Purification of cyclohexane |
| CN101544531A (en) * | 2009-05-06 | 2009-09-30 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent-normal hexane for scientific research |
| CN101570484A (en) * | 2009-06-15 | 2009-11-04 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethyl acetate |
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| CN101544531A (en) * | 2009-05-06 | 2009-09-30 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent-normal hexane for scientific research |
| CN101570484A (en) * | 2009-06-15 | 2009-11-04 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethyl acetate |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531820A (en) * | 2011-12-26 | 2012-07-04 | 天津市康科德科技有限公司 | Purification method of 2,2,4-trimethylpentane organic solvent of chromatographic grade |
| CN102755763A (en) * | 2012-07-18 | 2012-10-31 | 中国石油化工股份有限公司 | Method for purifying solvent for refining caprolactam crystal |
| CN102755763B (en) * | 2012-07-18 | 2015-08-19 | 中国石油化工股份有限公司 | A kind of method of purifying caprolactam crystal refining solvent |
| CN104744196A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Purifying method of high-purity organic solvent n-hexane |
| CN105085149A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent cyclohexane |
| CN105085139A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-heptane |
| CN105085137A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of high-purity organic solvent n-octane |
| CN105085139B (en) * | 2014-05-16 | 2017-11-10 | 上海星可高纯溶剂有限公司 | The method of purification of organic solvent normal heptane |
| CN105085149B (en) * | 2014-05-16 | 2018-01-16 | 上海星可高纯溶剂有限公司 | The method of purification of high-purity organic solvent hexamethylene |
| CN107501031A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatographically pure n-hexane and preparation method thereof, production system |
| CN107522588A (en) * | 2017-08-29 | 2017-12-29 | 湖北工程学院 | Chromatographically pure hexamethylene and preparation method thereof, production system |
| CN110713429A (en) * | 2019-10-29 | 2020-01-21 | 天津康科德医药化工有限公司 | Method for purifying chromatographically pure hexane |
| CN110713429B (en) * | 2019-10-29 | 2022-05-03 | 天津康科德医药化工有限公司 | Method for purifying chromatographically pure hexane |
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Application publication date: 20110504 |