CN102531820A - Purification method of 2,2,4-trimethylpentane organic solvent of chromatographic grade - Google Patents
Purification method of 2,2,4-trimethylpentane organic solvent of chromatographic grade Download PDFInfo
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- CN102531820A CN102531820A CN2011104403101A CN201110440310A CN102531820A CN 102531820 A CN102531820 A CN 102531820A CN 2011104403101 A CN2011104403101 A CN 2011104403101A CN 201110440310 A CN201110440310 A CN 201110440310A CN 102531820 A CN102531820 A CN 102531820A
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- pure isooctane
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- trimethylpentane
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Abstract
The invention relates to a purification method of a 2,2,4-trimethylpentane organic solvent of a chromatographic grade, comprising the following steps: removing alkene impurities in the raw material 2,2,4-trimethylpentane by allowing the raw material 2,2,4-trimethylpentane to pass through a silica gel column; drying by activated alumina and calcium hydride; rectifying; filtering; and packaging to obtain the 2,2,4-trimethylpentane product of a high performance liquid chromatography grade. The purification method of the invention employs 2,2,4-trimethylpentane with content of 99% as the raw material, silica gel as an adsorbent to adsorb and separate the alkene impurities in the raw material, and activated alumina and calcium hydride as drying agents to remove water in the raw material, obtains the 2,2,4-trimethylpentane product with purity of more than 99.7% and all qualified other chromatographic indexes by adsorbing, drying and rectifying and purifying, and has a recovery rate of more than 93% and a finished product ratio up to 92%.
Description
Technical field:
The invention belongs to chemical technology field, relate to the method for purification of organic solvent, especially a kind of method of purification of chromatographic grade organic solvent pure isooctane.
Background technology:
The chromatographically pure pure isooctane mainly is used as the stratographic analysis reference material, organic synthesis and solvent etc.
The pure isooctane reagent of selling on the market, content is merely about 99%, wherein contains impurity such as small amounts of olefins and water.This kind pure isooctane can not satisfy the needs of related scientific research test, and therefore, this kind pure isooctane must pass through further purification, and making its each item technical indicator all reach chromatographic grade standard could use.
At present, domestic data about pure isooctane purification aspect seldom, mainly be since in the pure isooctane content of impurity less, be difficult to further remove other impurity in the rectifying.Therefore, the present invention is directed to this technical barrier and propose effective solution.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, the method for purification of the chromatographic grade organic solvent pure isooctane that a kind of working method is simple, impurity is easily separated, product purity is high is provided.
The present invention is through following scheme implementation:
A kind of method of purification of chromatographic grade organic solvent pure isooctane, step is following:
(1) absorption: the flow velocity of the adsorption column of raw material pure isooctane through sorbent material is housed with 50mL-120mL/min adsorbed;
(2) drying: the pure isooctane after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.02%;
(3) rectifying: dried pure isooctane is squeezed into rectifying still carry out rectifying; Temperature is 150～300 ℃ at the bottom of the rectifying still, and fluid temperature is 120 ℃～150 ℃ in the still, and still top temperature is 99 ℃～100 ℃; Control reflux ratio 10: 1～9, backflow 2-3 hour, filtering with microporous membrane after the rectifying; Filtrating is the chromatographic grade pure isooctane.
And sorbent material is a silica gel in the described step (1), and particle diameter is 75 μ m～150 μ m.
And the material purity in the described step (1) is 99%.
And siccative is activated alumina and hydrolith in the described step (2).
And, need through toasting drying before the siccative activated alumina uses in the described step (2).
And, in said step (1) and (2) the dress post amount of sorbent material, siccative be post high 4/5.
And the specification of said dry post is identical with adsorption column.
And the flow velocity of pure isooctane is 80mL-150mL/min in the described step (2).
Advantage of the present invention and positively effect are:
1, the present invention with content be 99% 2; 2, the 4-trimethylpentane is raw material, carry out fractionation by adsorption with silica gel as sorbent material removes olefines impurity wherein, adopts activated alumina and hydrolith to remove moisture wherein as siccative; Obtain 2 of purity 99.7% through absorption, drying, rectification and purification; 2,4-trimethylpentane product, all other chromatogram indexs all reach requirement.
2, method of purification of the present invention is adsorbed the organic impurity of removing in the pure isooctane with silica gel; Promote pure isooctane content to 99.7%; Yield rate is increased to more than 90% by original 70%; Method is simple, impurity is easily separated, stable, save energy and reduce the cost, raise the efficiency, can be used for suitability for industrialized production, have remarkable economic efficiency.
3, the product of method of purification production of the present invention is through detecting the requirement that its each item index meets the chromatographically pure pure isooctane; They are 2 years old; 2,4-trimethylpentane content is greater than 99.7%, and the recovery is greater than 93%; Yield rate reaches 92%, and this product can satisfy the application demand of the user of performance liquid chromatography (HPLC) at aspects such as scientific experiments.
Embodiment:
Through specific embodiment the present invention is made further detailed description below, following examples are descriptive,
Not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of method of purification of chromatographic grade organic solvent pure isooctane, step is following:
(1) absorption: raw material pure isooctane (content is 99%) is promoted to the adsorption column top; The high 1.6M of adsorption column wherein, diameter 4.2cm, interior dress particle diameter are the silica gel absorber of 75 μ m～150 μ m; Dress post amount be post high 4/5; The pure isooctane raw material carries out adsorption-edulcoration with 50mL/min speed;
In this step, adsorption column interior 2,2; The 4-trimethylpentane fully contacts with silica gel absorber, removes olefines impurity, detects absorption fluid quality; Treat that the fluid check gets into next-step operation, and removes the absorption front-end volatiles near qualified (concrete technical requirement is seen table 1) back;
(2) drying: the effluent in the step (1) is got into dry post, and the specification of dry post and all same adsorption column of dress post amount are packed in the post through baking exsiccant activated alumina; Flow velocity is that 80mL/min detects dried 2; 2,4-trimethylpentane water cut, moisture controlled is≤0.02%;
Moisture content＞0.05% o'clock utilizes activated alumina in this step, removes the moisture in the pure isooctane after adsorbing, if carry out drying treatment after needing to change siccative again;
(3) rectifying: carry out rectifying with getting into rectifying still through dried pure isooctane in the step (2), add weight and be 0.2% hydrolith of solution.Use electrically heated, temperature is about 150 ℃ at the bottom of the rectifying still, and fluid temperature is 120 ℃ in the still, 99 ℃ ± 1 ℃ of still top temperature, and control reflux ratio 10: 1～4 refluxed 2 hours, detected qualified back adjusting reflux ratio and went out finished product at 10: 4.Finished product is behind 0.45 μ mPVDF filtering with microporous membrane, and the bottling sealing promptly gets the chromatographic grade pure isooctane that meets index request under nitrogen protection;
Greater than 99.7%, its front-end volatiles are for further processing through its purity of check.
Embodiment 2:
A kind of scientific research is with the method for purification of chromatographic grade organic solvent pure isooctane, and step is following:
(1) absorption: raw material pure isooctane (content is about 99%) is promoted to the adsorption column top; The high 1.6M of adsorption column; Diameter 4.2cm, interior dress be the amount of the silica gel absorber of particle diameter 75 μ m～150 μ m be post high 4/5,2; 2,4-trimethylpentane raw material carries out adsorption-edulcoration with 120mL/min speed;
In this step, adsorption column interior 2,2; The 4-trimethylpentane fully contacts with silica gel absorber, and olefines impurity is adsorbed, and detects absorption fluid quality; Treat that fluid (concrete technical requirement the see table 1) back that is up to the standards gets into next-step operation, and remove the absorption front-end volatiles;
(2) drying: just the effluent in the step (1) gets into dry post, and the specification of dry post and all same adsorption column of dress post amount are packed in the post through baking exsiccant activated alumina, and flow velocity is 150mL/min.Measure the water cut of dry back pure isooctane, moisture controlled is≤0.02%;
Moisture content＞0.05% o'clock utilize activated alumina to remove the moisture in the pure isooctane after adsorbing in this step, if carry out drying treatment after needing to change siccative again;
(3) rectifying: dry back pure isooctane in the step (2) is got into rectifying still carry out rectifying, add weight and be 1% hydrolith of solution.Use electrically heated, temperature is about 300 ℃ at the bottom of the control stainless steel still, and the pure isooctane fluid temperature is about 150 ℃ in the still, goes out 99 ℃ ± 1 ℃ of liquid temp, and the control reflux ratio refluxed 3 hours in 10: 5～9 fluids, detects qualified back adjusting reflux ratio and goes out finished product at 10: 9.Finished product is behind 0.45 μ mPVDF filtering with microporous membrane, and the bottling sealing promptly gets the chromatographic grade pure isooctane that meets index request under nitrogen protection;
Greater than 99.7%, its front-end volatiles are for further processing through its purity of check.
Effect detection:
Through purify the chromatographic grade pure isooctane; In ultraviolet wavelength 210nm～400nm scope (the quartzy cuvette of 1cm, water is made reference), absorbancy satisfies the index request in the table 1; Content is greater than 99.7%, moisture≤0.02%, and the recovery is greater than 93%; Yield rate reaches more than 92% approximately, and all other all meet desired value.
Table 1: the technical indicator of raw material, chromatographically pure pure isooctane
Claims (8)
1. the method for purification of a chromatographic grade organic solvent pure isooctane, it is characterized in that: step is following:
(1) absorption: the flow velocity of the adsorption column of raw material pure isooctane through sorbent material is housed with 50mL-120mL/min adsorbed;
(2) drying: the pure isooctane after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.02%;
(3) rectifying: dried pure isooctane is squeezed into rectifying still carry out rectifying; Temperature is 150～300 ℃ at the bottom of the rectifying still, and fluid temperature is 120 ℃～150 ℃ in the still, and still top temperature is 99 ℃～100 ℃; Control reflux ratio 10: 1～9, backflow 2-3 hour, filtering with microporous membrane after the rectifying; Filtrating is the chromatographic grade pure isooctane.
2. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: sorbent material is a silica gel in the described step (1), and particle diameter is 75 μ m～150 μ m.
3. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: the material purity in the described step (1) is 99%.
4. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: siccative is activated alumina and hydrolith in the described step (2).
5. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 4 is characterized in that: need through toasting drying before the siccative activated alumina uses in the described step (2).
6. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: in said step (1) and (2) the dress post amount of sorbent material, siccative be post high 4/5.
7. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: the specification of said dry post is identical with adsorption column.
8. the method for purification of a kind of chromatographic grade organic solvent pure isooctane according to claim 1 is characterized in that: the flow velocity of pure isooctane is 80mL-150mL/min in the described step (2).
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| CN2011104403101A CN102531820A (en) | 2011-12-26 | 2011-12-26 | Purification method of 2,2,4-trimethylpentane organic solvent of chromatographic grade |
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Citations (4)
| 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 |
| WO2010131585A1 (en) * | 2009-05-12 | 2010-11-18 | 和光純薬工業株式会社 | Method for purifying organic solvent |
| CN102040455A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of chromatographically pure organic solvent cyclohexane |
| CN102115356A (en) * | 2010-12-29 | 2011-07-06 | 天津市康科德科技有限公司 | Method for preparing chromatograph-grade normal heptane |
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Patent Citations (4)
| 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 |
| WO2010131585A1 (en) * | 2009-05-12 | 2010-11-18 | 和光純薬工業株式会社 | Method for purifying organic solvent |
| CN102040455A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of chromatographically pure organic solvent cyclohexane |
| CN102115356A (en) * | 2010-12-29 | 2011-07-06 | 天津市康科德科技有限公司 | Method for preparing chromatograph-grade normal heptane |
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Application publication date: 20120704 |