CN102070393A - Preparation method of high-efficiency liquid chromatographic-grade cyclohexane - Google Patents
Preparation method of high-efficiency liquid chromatographic-grade cyclohexane Download PDFInfo
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- CN102070393A CN102070393A CN2011100398829A CN201110039882A CN102070393A CN 102070393 A CN102070393 A CN 102070393A CN 2011100398829 A CN2011100398829 A CN 2011100398829A CN 201110039882 A CN201110039882 A CN 201110039882A CN 102070393 A CN102070393 A CN 102070393A
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Abstract
The invention relates to a preparation method of high-efficiency liquid chromatographic-grade cyclohexane, comprising the main steps of: adopting active carbon as an adsorbent, carrying out adsorption and separation to remove trace benzene and impurities with high ultraviolet absorption, drying with anhydrous calcium chloride to remove moisture, rectifying and purifying after drying, and removing trace impurities step by step. In the preparation method, cyclohexane with the content being 99.5% is taken as a raw material, a chromatographic-grade cyclohexane product with the purity being larger than 99.9% can be prepared after purification, and the yield is larger than 95%. Compared with the conventional method, the preparation method is high in product purity, simple and convenient to operate and stable in operation, and is suitable for industrialized production.
Description
Technical field
The invention belongs to chemical technology field, relate to the purification process of organic solvent, the preparation method of the pure level of especially a kind of high performance liquid chromatography 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.Be to remove trace impurity, we have carried out a large amount of experiments, have chosen the method for absorption, drying, rectifying, and to have replaced technological process complicated, and quality product can not reach the common process of scientific research requirement.
Domestic preparation method about high purity hexanaphthene reagent sets forth very few, mainly is owing to the content of impurity in the raw material hexanaphthene is very few, and general rectifying is difficult to small amount of impurities is removed, and therefore, The present invention be directed to this technical barrier and proposes effective solution.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing production technology, a kind of method of utilizing the activated carbon of sorbent removal of impurities, using the dry hexanaphthene of Calcium Chloride Powder Anhydrous 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.
Specific embodiments of the present invention is:
A kind of preparation method of high-efficient liquid phase color spectrum level hexanaphthene, the step of preparation is as follows:
(1) the raw material hexanaphthene is adsorbed by the adsorption tower that activated carbon of sorbent is housed;
(2) hexanaphthene after will adsorbing carries out drying with the siccative Calcium Chloride Powder Anhydrous, 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: 2～8, the rectifying after-filtration, promptly obtains high-efficient liquid phase color spectrum level hexanaphthene.
And, described raw material hexanaphthene with the 50-120mL/min velocity flow through the sorbent material tower.
And described sorbent material is a gac, and activated carbon particle size is 0.35mm～0.49mm.
Advantage of the present invention and positively effect are:
1, the present invention takes the method for rectifying after activated carbon of sorbent absorption, the Calcium Chloride Powder Anhydrous drying progressively to remove wherein trace impurity, and is simple and easy to do, makes the rectifying time save about 3～5 hours, and yield rate brings up to 95% by original 70%～80%; Compare with ordinary method, 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.
2, the present invention can obtain the chromatogram hexanaphthene product of purity 〉=99.9%, and yield 〉=95%, the reagent after the purification 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 preparation method of high-efficient liquid phase color spectrum level 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 activated carbon of sorbent be 4/5 of tower height, the hexanaphthene raw material adsorbs with 50mL/min speed; In tower, hexanaphthene fully contacts with activated carbon of sorbent, 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 Calcium Chloride Powder Anhydrous of packing into, Calcium Chloride Powder Anhydrous contact the moisture that sponges wherein with hexanaphthene, measure the water content of dry back hexanaphthene, 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: 2～5 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 preparation method of high-efficient liquid phase color spectrum level 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 activated carbon of sorbent be 4/5 of tower height, the hexanaphthene raw material adsorbs with 120mL/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 Calcium Chloride Powder Anhydrous 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 high-efficient liquid phase color spectrum level hexanaphthene for preparing, (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%, and moisture is less than 0.02%, and the rate of recovery is greater than 95%, yield rate reaches more than 95% approximately, and all other indexs all meet the requirements.
Table 1: the index of chromatographic grade hexanaphthene
Claims (3)
1. the preparation method of a high-efficient liquid phase color spectrum level hexanaphthene, it is characterized in that: the step of preparation is as follows:
(1) the raw material hexanaphthene is adsorbed by the adsorption tower that activated carbon of sorbent is housed;
(2) hexanaphthene after will adsorbing carries out drying with the siccative Calcium Chloride Powder Anhydrous, 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: 2～8, the rectifying after-filtration, promptly obtains high-efficient liquid phase color spectrum level hexanaphthene.
2. the preparation method of high-efficient liquid phase color spectrum level hexanaphthene according to claim 1 is characterized in that: described raw material hexanaphthene with the 50-120mL/min velocity flow through the sorbent material tower.
3. the preparation method of high-efficient liquid phase color spectrum level hexanaphthene according to claim 1 is characterized in that: described sorbent material is a gac, and activated carbon particle size is 0.35mm～0.49mm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108614061A (en) * | 2018-07-02 | 2018-10-02 | 山东师范大学 | A method of plasticiser in removal absolute ethyl alcohol and hexamethylene |
| CN112939720A (en) * | 2021-03-04 | 2021-06-11 | 滁州市润达溶剂有限公司 | Cyclohexane purification process |
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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 |
| CN101570468A (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 ethanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN101570468A (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 ethanol |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108614061A (en) * | 2018-07-02 | 2018-10-02 | 山东师范大学 | A method of plasticiser in removal absolute ethyl alcohol and hexamethylene |
| CN112939720A (en) * | 2021-03-04 | 2021-06-11 | 滁州市润达溶剂有限公司 | Cyclohexane purification process |
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Application publication date: 20110525 |