CN102731251A - Purification method of highly pure organic solvent n-butanol - Google Patents
Purification method of highly pure organic solvent n-butanol Download PDFInfo
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- CN102731251A CN102731251A CN2012102322000A CN201210232200A CN102731251A CN 102731251 A CN102731251 A CN 102731251A CN 2012102322000 A CN2012102322000 A CN 2012102322000A CN 201210232200 A CN201210232200 A CN 201210232200A CN 102731251 A CN102731251 A CN 102731251A
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- propyl carbinol
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- butanol
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Abstract
The invention relates to a purification method of highly pure organic solvent n-butanol. The method comprises the following steps of: removing most aldehyde, ketone and ester impurities in the raw material n-butanol by adsorption of silica gel and a diatomite column; drying and dewatering by a drying agent of anhydrous magnesium sulphate or anhydrous potassium carbonate; rectifying; filtering; and packing to obtain the highly pure organic solvent n-butanol. The purification method provided by the invention can obtain the highly pure organic solvent n-butanol with the purity over 99.9%; the yield of the n-butanol is more than 92%; the qualified rate of the n-butanol is more than 92%; the application need of users of highly pure organic solvent n-butanol (HPLC) (high performance liquid chromatography) in the scientific research and the subject research can be satisfied; compared with the traditional methods, the n-butanol obtained by the method provided by the invention is high in the purity; the operation is simple; the quality of the product is stable, and thus the method is applied to the 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 propyl carbinol.
Background technology
Propyl carbinol mainly as the extraction agent of solvent, dewatering agent, non-emulsifying agent and grease, spices medicine, hormone etc., as reducing agent, solubility promoter, is used as standard substance and the high purity reagent in scientific experiment in chemical industry in stratographic analysis.The content of conventional propyl carbinol reagent is about 99.5%, and wherein major impurity is water and small amounts of aldehyde, ketone, ester class organic impurity.This kind propyl carbinol can not satisfy high-purity organic solvent propyl carbinol user's demand, so this kind propyl carbinol must pass through and be further purified, and the standard that makes its each item technical indicator all reach high-purity organic solvent could be used.
At present, domestic purification process about the chromatogram propyl carbinol is reported seldom.
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 purification process of high-purity organic solvent propyl carbinol, this purification process has characteristics such as technology is simple, steady quality, product purity height.
The present invention is through following scheme implementation:
A kind of purification process of high-purity organic solvent propyl carbinol, step is following:
(1) with the raw material propyl carbinol with the 60-120mL/min velocity flow through the adsorption column of sorbent material is housed;
(2) propyl carbinol after will adsorbing carries out drying through dry post, and measures water cut, and qualified moisture is controlled at≤and 0.05%;
(3) water cut after the drying is carried out rectifying at the propyl carbinol of acceptability limit, temperature is 180 ~ 300 ℃ at the bottom of the rectifying still, and the propyl carbinol fluid temperature is 120 ℃ ~ 150 ℃ in the still, 116 ℃ ~ 118 ℃ of still top temperature, control reflux ratio 10:3 ~ 8;
(4) rectifying liquid promptly obtains high-purity organic solvent propyl carbinol product through filtering.
And, the high 1.2M of adsorption column in the said step (1), diameter 3.8cm is equipped with silica gel, zeyssatite respectively in two posts, its particle diameter is respectively 0.5 ~ 1.0mm and 0.3 ~ 0.8mm, two posts series connection, the amount of sorbent material be post high 4/5.
And the siccative in the said dry post is anhydrous magnesium sulfate or Anhydrous potassium carbonate.
Advantage of the present invention and positively effect are:
1, to be about 99.5% propyl carbinol with content be raw material to this purification process, carries out fractionation by adsorption with silica gel, zeyssatite as sorbent material, removes most of aldehyde, ketone, ester class organic impurity; Adopt anhydrous magnesium sulfate or Anhydrous potassium carbonate to remove moisture wherein as siccative, obtain purity greater than 99.9% propyl carbinol product through absorption, dry, rectifying purifying, this purification process is simple, and product purity is high, and is stable, can be used for large-scale production.
2, this purification process with silica gel, zeyssatite as sorbent material adsorb, anhydrous magnesium sulfate or Anhydrous potassium carbonate be dry; Can promote propyl carbinol content extremely greater than 99.9%; All other indexs can both reach the requirement of high-purity organic solvent propyl carbinol, and yield rate is increased to more than 90% by original 60%.Save manpower, reduce energy consumption, more be applicable to large-scale production and application, have remarkable economic efficiency.
3, the product of this purification process production is through detecting the requirement that its each item index meets the high-purity organic solvent propyl carbinol; Its propyl carbinol content is greater than 99.9%; The recovery is greater than 92%, and yield rate reaches 92%, can satisfy the demand of the client of use high-purity organic solvent propyl carbinol 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 purification process of high-purity organic solvent propyl carbinol, step is following:
(1) raw material propyl carbinol (content is about 99.5%) is promoted to the adsorption column top, the propyl carbinol raw material adsorbs with 60mL/min speed; The high 1.2M of adsorption column wherein, diameter 3.8cm is equipped with silica gel, zeyssatite respectively in two posts, its particle diameter is respectively 0.5 ~ 1.0mm and 0.3mm ~ 0.8mm, the series connection of two posts, the amount of sorbent material be post high 4/5.In post, propyl carbinol fully contacts with silica gel, diatomite adsorbant, and most of aldehyde, ketone, ester class organic impurity are removed in absorption, waits to adsorb fluid and checks near after qualified (concrete technical requirement is seen table 1), gets into next-step operation, and removes the absorption front-end volatiles.
(2) the effusive propyl carbinol of above-mentioned adsorption column is got into dry post, the high 1.2M of post, diameter 3.8cm packs into through baking exsiccant anhydrous magnesium sulfate, detects the water cut of dry back propyl carbinol, 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.
(3) flow to rectifying still through dried propyl carbinol and carry out rectifying above-mentioned, be further drying, the amount that adds hydrolith in the still is about 0.3% of propyl carbinol quality; Utilize electrically heated, temperature is about 180 ℃ at the bottom of the control rectifying still, and the propyl carbinol fluid temperature is about 120 ℃ in the still, 116 ℃ ± 1 ℃ of still top temperature, control reflux ratio 10:3 ~ 5 fluids.
(4) finished product is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing promptly obtains qualified high-purity organic solvent propyl carbinol product (purity is greater than 99.9%) under nitrogen protection, and its front-end volatiles are handled in addition.
Embodiment 2:
A kind of purification process of high-purity organic solvent propyl carbinol, step is following:
(1) raw material propyl carbinol (content is about 99.5%) is promoted to the adsorption column top, the propyl carbinol raw material adsorbs with 120mL/min speed; The high 1.2M of adsorption column wherein, diameter 3.8cm is equipped with silica gel, zeyssatite respectively in two posts, its particle diameter is respectively 0.5～1.0mm and 0.3mm ~ 0.8mm, the series connection of two posts, the amount of sorbent material be post high 4/5.In post, propyl carbinol fully contacts with silica gel, diatomite adsorbant, and most of aldehyde, ketone, ester class organic impurity are removed in absorption, waits to adsorb fluid and checks near after qualified (concrete technical requirement is seen table 1), gets into next-step operation, and removes the absorption front-end volatiles.
(2) the effusive propyl carbinol of above-mentioned adsorption column is got into dry post; The high 1.2M of post, diameter 3.8cm packs into through baking exsiccant Anhydrous potassium carbonate; Detect the water cut of dry back propyl carbinol; 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.
(3) flow to rectifying still through dried propyl carbinol and carry out rectifying above-mentioned, be further drying, the amount that adds hydrolith in the still is about 0.3% of propyl carbinol quality.Utilize electrically heated, temperature is about 300 ℃ at the bottom of the control rectifying still, and the propyl carbinol fluid temperature is about 150 ℃ in the still, 118 ℃ ± 1 ℃ of still top temperature, control reflux ratio 10:6 ~ 8 fluids.
(4) finished product is behind 0.45 μ m filtering with microporous membrane, and the bottling sealing promptly obtains qualified high-purity organic solvent propyl carbinol product (purity is greater than 99.9%) under nitrogen protection, and its front-end volatiles are handled in addition.
Effect detection:
Purified high-purity organic solvent propyl carbinol is in ultraviolet wavelength 210nm ~ 400nm scope (the quartzy cuvette of 1cm, water is made reference); Absorbancy satisfies the index request in the table 1, and content is greater than 99.9%, moisture≤0.05%; The recovery is greater than 92%; Yield rate reaches more than 92% approximately, and all other all meet desired value, can satisfy the customer demand of high-purity organic solvent propyl carbinol.
Table 1: the technical indicator of raw material, high-purity organic solvent propyl carbinol
Claims (3)
1. the purification process of a high-purity organic solvent propyl carbinol, it is characterized in that: the step of purification process is following:
(1) with the raw material propyl carbinol with the 60-120mL/min velocity flow through the adsorption column of sorbent material is housed;
(2) propyl carbinol after will adsorbing carries out drying through dry post, and measures water cut, and qualified moisture is controlled at≤and 0.05%;
(3) water cut after the drying is carried out rectifying at the propyl carbinol of acceptability limit, temperature is 180 ~ 300 ℃ at the bottom of the rectifying still, and the propyl carbinol fluid temperature is 120 ℃ ~ 150 ℃ in the still, 116 ℃ ~ 118 ℃ of still top temperature, control reflux ratio 10:3 ~ 8;
(4) rectifying liquid promptly obtains high-purity organic solvent propyl carbinol product through filtering.
2. the purification process of high-purity organic solvent propyl carbinol according to claim 1; It is characterized in that: the high 1.2M of adsorption column in the said step (1); Diameter 3.8cm is equipped with silica gel, zeyssatite respectively in two posts, its particle diameter is respectively 0.5 ~ 1.0mm and 0.3 ~ 0.8mm; Two posts series connection, the amount of sorbent material be post high 4/5.
3. the purification process of a kind of high-purity organic solvent propyl carbinol according to claim 1 is characterized in that: the siccative in the said dry post is anhydrous magnesium sulfate or Anhydrous potassium carbonate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085173A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic grade n-butanol |
| CN114507119A (en) * | 2021-12-31 | 2022-05-17 | 江苏天晟药业股份有限公司 | Method for purifying n-butanol solvent in diammonium glycyrrhizinate production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN102432428A (en) * | 2011-12-26 | 2012-05-02 | 天津市康科德科技有限公司 | Method for purifying chromatographically pure organic solvent tert-butyl alcohol |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN102432428A (en) * | 2011-12-26 | 2012-05-02 | 天津市康科德科技有限公司 | Method for purifying chromatographically pure organic solvent tert-butyl alcohol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085173A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic grade n-butanol |
| CN114507119A (en) * | 2021-12-31 | 2022-05-17 | 江苏天晟药业股份有限公司 | Method for purifying n-butanol solvent in diammonium glycyrrhizinate production |
| CN114507119B (en) * | 2021-12-31 | 2024-04-26 | 江苏天晟药业股份有限公司 | Purification method of n-butanol solvent in production of diammonium glycyrrhizinate |
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