CN102746115A - Purification method for high-purity organic solvent normal propyl alcohol - Google Patents
Purification method for high-purity organic solvent normal propyl alcohol Download PDFInfo
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- CN102746115A CN102746115A CN2012102487677A CN201210248767A CN102746115A CN 102746115 A CN102746115 A CN 102746115A CN 2012102487677 A CN2012102487677 A CN 2012102487677A CN 201210248767 A CN201210248767 A CN 201210248767A CN 102746115 A CN102746115 A CN 102746115A
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- propyl alcohol
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Abstract
The invention relates to a purification method for high-purity organic solvent normal propyl alcohol. The method includes steps: subjecting raw normal propyl alcohol to removal of high ultraviolet absorption impurities by the aid of activated carbon, utilizing desiccants such as anhydrous calcium sulfate or calcium hydride for drying and dehydration, rectifying, filtering and packaging to obtain the high-purity organic solvent normal propyl alcohol. By the purification method for the high-purity organic solvent normal propyl alcohol, chromatographic-grade normal propyl alcohol products with the purity higher than 99.8% can be obtained, the yield is higher than 95%, the acceptance rate is higher than 93%, and application requirements of users in aspects of scientific researches, subject studies and the like of the high-purity organic solvent (HPLC) normal propyl alcohol can be met. In addition, compared with conventional methods, the purification method for the high-purity organic solvent normal propyl alcohol is high in product purity, simple and convenient to operate and stable in product quality and can be used for large-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 n-propyl alcohol.
Background technology
N-propyl alcohol mainly as solvent, the clean-out system of plant oil, tree elastomer, resin and Mierocrystalline cellulose etc., is used as raw material in organic synthesis, in stratographic analysis, be used as standard substance and the high purity reagent in scientific experiment.Conventional n-propyl alcohol reagent, its n-propyl alcohol content is about 99.1%, and major impurity is water and vinyl carbinol.This kind n-propyl alcohol can not satisfy high-purity organic solvent n-propyl alcohol user's demand, must be through further purifying, and making its each item technical indicator all reach chromatographic grade standard could use.
At present, domestic method of purification about the chromatogram n-propyl alcohol is reported seldom, mainly is that general method is difficult to remove because the impurity level in the commercially available n-propyl alcohol reagent is few.
Through retrieval, do not find the publication document relevant with application of the present invention yet.
Summary of the invention
The object of the present invention is to provide a kind of method of purification of high-purity organic solvent n-propyl alcohol, this method of purification has characteristics such as technology is simple, steady quality, product purity height.
The present invention is through following scheme implementation:
A kind of method of purification of high-purity organic solvent n-propyl alcohol, step is following:
With the raw material n-propyl alcohol with the 40-100mL/min velocity flow through active carbon adsorption column;
⑵ the n-propyl alcohol after will adsorb gets into dry post and carries out drying, and measures water cut, and qualified moisture is controlled at≤and 0.05%;
With drying after water cut carry out rectifying at the n-propyl alcohol of acceptability limit, temperature is 150 ~ 300 ℃ at the bottom of the rectifying still, the n-propyl alcohol fluid temperature is 100 ℃ ~ 140 ℃ in the still, 97 ℃ ~ 98 ℃ of still top temperature, control of reflux ratio 10:2 ~ 9;
⑷ rectifying liquid is through filtering with microporous membrane, and the bottling sealing promptly obtains high-purity organic solvent n-propyl alcohol product under nitrogen protection.
And the particle diameter of said activated carbon of sorbent is 0.4mm ~ 0.8mm, dress post amount be post high 4/5.
And the siccative in the said dry post is anhydrous calciumsulphate or hydrolith.
Advantage of the present invention and positively effect are:
1, to be about 99.1% n-propyl alcohol with content be raw material to this method of purification, carry out fractionation by adsorption with gac as sorbent material removes the wherein high impurity of uv-absorbing; Adopt anhydrous calciumsulphate or hydrolith to remove moisture wherein as siccative; Obtain purity greater than 99.8% n-propyl alcohol product through absorption, dry, rectification and purification, this method of purification is simple, and product purity is high; Stable, can be used for large-scale production.
2, this method of purification is removed the organic impurity in the n-propyl alcohol with charcoal absorption, and anhydrous calciumsulphate or hydrolith are dry, promotes n-propyl alcohol content extremely greater than 99.8%; All other chromatogram indexs all reach requirement; Yield rate is increased to more than 90% by original 70%, saves manpower, reduces energy consumption; More be applicable to large-scale production and application, have remarkable economic efficiency.
3, the product of this method of purification production is through detecting the requirement that its each item index meets the high-purity organic solvent n-propyl alcohol; Its n-propyl alcohol content is greater than 99.8%; The recovery is greater than 93%, and yield rate reaches 93%, can satisfy the demand of the client of use high-purity organic solvent n-propyl alcohol at aspects such as scientific experiments.
Specific embodiment
Through specific embodiment the present invention is made further detailed description below, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of method of purification of high-purity organic solvent n-propyl alcohol, step is following:
⑴ be promoted to adsorption column top with raw material n-propyl alcohol (content is about 99.1%), the n-propyl alcohol raw material with the 40mL/min velocity flow through adsorption column.The high 1.6M of adsorption column, diameter 4.2cm, in it amount of dress acticarbon be post high 4/5, the particle diameter of gac is 0.4mm ~ 0.8mm.In adsorption column, n-propyl alcohol fully contacts with acticarbon, falls the high organic impurity of ultraviolet with absorption.After waiting to adsorb fluid check approaching qualified (concrete technical requirement is seen table 1), get into next-step operation, be further purified and remove the absorption front-end volatiles.
⑵ get into dry post with the effusive n-propyl alcohol of above-mentioned adsorption column, the high 1.6M of post, and diameter 4.2cm packs into through baking exsiccant anhydrous calciumsulphate, detects the water cut of n-propyl alcohol after drying, and moisture controlled is≤0.05%; If moisture content is carried out drying treatment after greater than 0.1% o'clock, needing to change siccative again.
⑶ carry out rectifying with above-mentioned through dried n-propyl alcohol inflow rectifying still, is further drying, adds anhydrous calciumsulphate in the still; The amount that adds anhydrous calciumsulphate is 0.1 ~ 0.5% of a n-propyl alcohol quality; Utilize electrically heated, temperature is about 150 ℃ at the bottom of the control rectifying still, and the n-propyl alcohol fluid temperature is about 100 ℃ in the still; 97 ℃ ~ 98 ℃ of still top temperature, control reflux ratio 10:2 ~ 5 fluids.
⑷ finished product is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing promptly obtains qualified high-purity organic solvent n-propyl alcohol product (purity is greater than 99.8%) under nitrogen protection, and its front-end volatiles are handled in addition.
Embodiment 2:
A kind of method of purification of high-purity organic solvent n-propyl alcohol, step is following:
⑴ be promoted to the adsorption column top with raw material n-propyl alcohol (content is about 99.1%), and the n-propyl alcohol raw material adsorbs with 100mL/min speed.The high 1.6M of adsorption column, diameter 4.2cm, the amount of interior dress acticarbon be post high 4/5, the particle diameter of gac is 0.4mm ~ 0.8mm.Wait to adsorb the fluid check and get into next-step operation, be further purified and remove the high absorption front-end volatiles of impurity near qualified back;
⑵ get into dry post with the effluent of above-mentioned adsorption column, tower height 1.6M, and diameter 4.2cm, the hydrolith of packing into, the water cut of the dry back of measurement n-propyl alcohol, moisture controlled are≤0.05%, and the qualified back of water cut gets into next-step operation; When moisture content greater than 0.1% the time, carry out drying treatment again after needing to change siccative.
⑶ be further drying with above-mentioned through dry back n-propyl alcohol inflow rectifying still, adds hydrolith in the still; The amount that adds hydrolith is 0.1 ~ 0.5% of a n-propyl alcohol quality; Utilize electrically heated, temperature is about 300 ℃ at the bottom of the still, and the n-propyl alcohol fluid temperature is about 140 ℃ in the still; Go out about 97 ℃ ~ 98 ℃ of liquid temp, the control reflux ratio is in 10:6 ~ 9 fluids.
⑷ finished product is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing promptly obtains high-purity organic solvent n-propyl alcohol product (purity is greater than 99.8%) under nitrogen protection, and its front-end volatiles are handled in addition.
Effect detection:
Through the high-purity organic solvent n-propyl alcohol of purifying, 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 99.8%, moisture≤0.05%, and the recovery is greater than 93%; Yield rate reaches more than 93% approximately, and all other require all to meet desired value.
Table 1: the technical indicator of raw material, high-purity n-propyl alcohol
Claims (3)
1. the method for purification of a high-purity organic solvent n-propyl alcohol, it is characterized in that: the step of purification is following:
With the raw material n-propyl alcohol with the 40-100mL/min velocity flow through active carbon adsorption column;
⑵ the n-propyl alcohol after will adsorb gets into dry post and carries out drying, and measures water cut, and qualified moisture is controlled at≤and 0.05%;
With drying after water cut carry out rectifying at the n-propyl alcohol of acceptability limit, temperature is 150 ~ 300 ℃ at the bottom of the rectifying still, the n-propyl alcohol fluid temperature is 100 ℃ ~ 140 ℃ in the still, 97 ℃ ~ 98 ℃ of still top temperature, control of reflux ratio 10:2 ~ 9;
⑷ rectifying liquid is through filtering with microporous membrane, and the bottling sealing promptly obtains high-purity organic solvent n-propyl alcohol product under nitrogen protection.
2. the method for purification of high-purity organic solvent n-propyl alcohol according to claim 1 is characterized in that: the particle diameter of said activated carbon of sorbent is 0.4mm ~ 0.8mm, dress post amount be post high 4/5.
3. the method for purification of high-purity organic solvent n-propyl alcohol according to claim 1 is characterized in that: the siccative in the said dry post is anhydrous calciumsulphate or hydrolith.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012102487677A CN102746115A (en) | 2012-07-18 | 2012-07-18 | Purification method for high-purity organic solvent normal propyl alcohol |
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| CN2012102487677A CN102746115A (en) | 2012-07-18 | 2012-07-18 | Purification method for high-purity organic solvent normal propyl alcohol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744213A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Method for purifying chromatographic grade isopropanol |
| CN105085184A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of isopropyl alcohol for liquid chromatography-mass spectrometer |
| CN107337583A (en) * | 2017-08-29 | 2017-11-10 | 湖北工程学院 | Chromatographically pure normal propyl alcohol and preparation method thereof, production system |
-
2012
- 2012-07-18 CN CN2012102487677A patent/CN102746115A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744213A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Method for purifying chromatographic grade isopropanol |
| CN105085184A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of isopropyl alcohol for liquid chromatography-mass spectrometer |
| CN107337583A (en) * | 2017-08-29 | 2017-11-10 | 湖北工程学院 | Chromatographically pure normal propyl alcohol and preparation method thereof, production system |
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Application publication date: 20121024 |