CN102115356A - Method for preparing chromatograph-grade normal heptane - Google Patents
Method for preparing chromatograph-grade normal heptane Download PDFInfo
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- CN102115356A CN102115356A CN2010106119586A CN201010611958A CN102115356A CN 102115356 A CN102115356 A CN 102115356A CN 2010106119586 A CN2010106119586 A CN 2010106119586A CN 201010611958 A CN201010611958 A CN 201010611958A CN 102115356 A CN102115356 A CN 102115356A
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Abstract
The invention relates to a method for preparing chromatograph-grade normal heptane. The method comprises the following steps of: removing alkanes and cycloalkanes compounds with similar boiling points through an adsorption column and removing carbonyl compounds with a diatomite column; dewatering with a drier; refining, purifying and filtering to obtain a qualified chromatograph-grade normal heptane product. By utilizing the difference between the normal heptane and the impurity thereof in properties, the process flows of absorption, drying and distillation are adopted, and the normal heptane and certain impurities thereof are separated and purified to reach the indexes (shown in a graph 1) of the chromatograph-grade normal heptane and the chromatographic net yield higher than 95 percent so as to form the mass production of the chromatograph-grade normal heptane.
Description
Technical field
The invention belongs to the chemical reagent field, relate to the purifying of organic reagent, especially a kind of preparation method of chromatographic grade normal heptane.
Background technology
Normal heptane is widely used in producing coating, dyestuff, pigment, printing ink, tackiness agent, medicine, agricultural chemicals, food, fodder additives, essence and flavoring agent, makeup; Pure standard substance, the standard of octane number determination, the solvent of tasting with discrimination normal heptane as stratographic analysis, and organic synthesis, the preparation of experiment reagent etc.In recent years, because science and technology development, the experimental study problem is on the increase, and existing high-purity chromatorgaphy reagent mainly is by import, though homemade high purity reagent has production, quality
Instability, and do not satisfy the demand of scientific and technological high speed development, therefore, preparation method, the especially preparation method of chromatographic grade normal heptane of research high-purity organic solvent have important practical significance alternative again import to China's development in science and technology.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of small amount of impurities, product purity of being difficult in the normal heptane remove can effectively removed to reach the chromatographic grade index, and the preparation method of the simple chromatographic grade normal heptane of technology.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of chromatographic grade normal heptane, the step of preparation is as follows:
(1) feed n-heptane is promoted to the silica gel adsorption column top, utilizes gravity to flow in the post, control flow velocity 50mL～80mL/min removes the initial flow fluid, and fluid is detected;
(2) qualified fluid be will detect and diatomite adsorption post, flow velocity 50mL～80mL/min flowed into;
(3) the fluid drying post with step (2) carries out drying, dry fluid control moisture content 0.01%～0.05%;
(4) dried fluid is squeezed into reactor rectifying, 140 ℃～200 ℃ of control Heating temperatures, the normal heptane fluid temperature is 100 ℃～110 ℃ in the still, goes out 98 ℃～99 ℃ of liquid temps; Reflux ratio 10: 5～8, regulate reflux ratio to 10: 12～15, obtain chromatographic grade normal heptane product at last.
And the purity of described feed n-heptane is about 98%.
And the length of described adsorption column is 1.5m, internal diameter 3.2cm, and the amount of dress sorbent material is 4/5 of a column length.
Advantage of the present invention and positively effect are:
1, the present invention utilizes the difference on normal heptane and the contaminant characteristics wherein, adopt the production method of absorption after drying, rectifying, normal heptane is separated with small amount of impurities wherein, the back product of purifying can reach chromatographic grade normal heptane index (seeing Table 1), further purify through rectifying, chromatographically pure normal heptane productive rate can form the scale production of chromatographic grade normal heptane greater than 95%.
2, the present invention takes to adsorb, method dry, rectifying removes wherein impurity, obtain qualified product by the processing condition rectifying of determining, can obtain the chromatographic grade normal heptane product of purity 〉=99%, compare the product purity height of this law preparation with ordinary method, equipment configuration is simple, and is stable.
Embodiment
Below content of the present invention is further elaborated by following embodiment, but these embodiment do not limit protection scope of the present invention.
A kind of preparation method of chromatographic grade normal heptane, step is as follows:
(1) purity is about 98% feed n-heptane and is promoted to the silica gel adsorption column top, the specification of adsorption column is: length 1.5m, internal diameter 3.2cm, dress silica gel amount is 4/5 of a column length, utilizes gravity to flow in the post, control flow velocity 50mL～80mL/min, organic solvent is fully contacted with silica gel, and absorption alkane and aromatic hydrocarbon impurity wherein, remove initial flow fluid (about 200～500 milliliters), the impurity band in the silica gel can be come out during because of beginning,, fluid is detected.
(2) will detect qualified normal heptane fluid and flow into the diatomite adsorption post, this diatomite adsorption post is identical with silica gel adsorption column, utilize the diatomite adsorption post to contact with organic solvent, can adsorption of carbonyl compounds etc. impurity and separating with it, flow velocity 50mL～80mL/min, fluid detects absorbancy near index.
To employed adsorption column (silica gel, diatomite) in above two steps, the applicant has carried out test of many times.The result shows, adopts two kinds of sorbent material associating results of use better.After the absorption of two-stage adsorption column, the content of normal heptane 〉=99%.
(3) the normal heptane fluid drying post with step (2) carries out drying, siccative in the dry post is Calcium Chloride Powder Anhydrous or hydrolith, dry fluid water content 0.01%～0.05% is considered as siccative by water saturation greater than 0.05%, carries out drying again after changing siccative.
After Calcium Chloride Powder Anhydrous or hydrolith drying, moisture reaches 0.01%～0.05%.
(4) dried fluid is squeezed into reactor rectifying, utilize electrically heated, 140 ℃～200 ℃ of control Heating temperatures, the normal heptane fluid temperature is 100 ℃～110 ℃ in the still, goes out 98 ℃～99 ℃ of liquid temps; Reflux ratio 10: 5～8, regulating reflux ratio gradually is 10: 12～15, obtains chromatographic grade normal heptane product at last;
By the processing condition rectifying of determining, control rectification temperature and reflux ratio, behind the removal front-end volatiles, the normal heptane of preparing all meets the chromatogram index request.
(5) qualified back finished product stores under nitrogen protection with 0.45 μ m filtering with microporous membrane, bottling.
Effect detection:
The chromatographic grade normal heptane finished product of preparing, (the quartzy cuvette of 1cm in ultraviolet wavelength 197nm～400nm scope, water is made reference), absorbancy satisfies the index request in the table 1, content is greater than 99.0%, moisture≤0.01%, and the rate of recovery is greater than 95%, yield rate reaches more than 95% approximately, and other index all reaches requirement.
Table 1 chromatographic grade normal heptane technical indicator
Claims (3)
1. the preparation method of a chromatographic grade normal heptane, it is characterized in that: the step of preparation is as follows:
(1) feed n-heptane is promoted to the silica gel adsorption column top, utilizes gravity to flow in the post, control flow velocity 50mL～80mL/min removes the initial flow fluid, and fluid is detected;
(2) qualified fluid be will detect and diatomite adsorption post, flow velocity 50mL～80mL/min flowed into;
(3) the fluid drying post with step (2) carries out drying, dry fluid control moisture content 0.01%～0.05%;
(4) dried fluid is squeezed into reactor rectifying, 140 ℃～200 ℃ of control Heating temperatures, the normal heptane fluid temperature is 100 ℃～110 ℃ in the still, goes out 98 ℃～99 ℃ of liquid temps; Reflux ratio 10: 5～8, regulate reflux ratio to 10: 12～15, obtain chromatographic grade normal heptane product at last.
2. the preparation method of chromatographic grade normal heptane according to claim 1 is characterized in that: the purity of described feed n-heptane is about 98%.
3. the preparation method of chromatographic grade normal heptane according to claim 1 is characterized in that: the length of described adsorption column is 1.5m, internal diameter 3.2cm, and the amount of dress sorbent material is 4/5 of a column length.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010106119586A CN102115356A (en) | 2010-12-29 | 2010-12-29 | Method for preparing chromatograph-grade normal heptane |
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| CN2010106119586A CN102115356A (en) | 2010-12-29 | 2010-12-29 | Method for preparing chromatograph-grade normal heptane |
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Cited By (6)
| 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 |
| 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 |
| CN105085138A (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-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 |
| CN107011111A (en) * | 2017-05-06 | 2017-08-04 | 洛阳和梦科技有限公司 | The method for removing micro aromatic hydrocarbons in heptane |
| CN107501032A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatographically pure normal heptane and preparation method thereof, production system |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2010
- 2010-12-29 CN CN2010106119586A patent/CN102115356A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| 叶锡麟 等: "自溶液中的吸附IX硅胶自环己烷中吸附苯、萘、蒽、菲的热力学研究", 《化学学报》 * |
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 |
| 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 |
| CN104744196B (en) * | 2013-12-31 | 2017-11-10 | 上海星可高纯溶剂有限公司 | The method of purification of organic solvent-normal hexane |
| CN105085138A (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-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 |
| CN105085137B (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 octane |
| CN105085138B (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 hexane |
| CN107011111A (en) * | 2017-05-06 | 2017-08-04 | 洛阳和梦科技有限公司 | The method for removing micro aromatic hydrocarbons in heptane |
| CN107501032A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatographically pure normal heptane and preparation method thereof, production system |
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Application publication date: 20110706 |