CN102731251B - 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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- CN102731251B CN102731251B CN201210232200.0A CN201210232200A CN102731251B CN 102731251 B CN102731251 B CN 102731251B CN 201210232200 A CN201210232200 A CN 201210232200A CN 102731251 B CN102731251 B CN 102731251B
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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 approximately 99.5% of conventional propyl carbinol reagent, wherein major impurity is water and a small amount of aldehyde, ketone, ester class organic impurity.This kind of propyl carbinol can not meet high-purity organic solvent propyl carbinol user's demand, and therefore this kind of propyl carbinol must be through being further purified, and the standard that makes its all technical all reach high-purity organic solvent could be used.
At present, the domestic report of the purification process about chromatogram propyl carbinol seldom.
By retrieval, do not find patent document related with the present patent application 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 that technique is simple, steady quality, product purity high.
The present invention is by following scheme implementation:
A purification process for high-purity organic solvent propyl carbinol, step is as follows:
(1) raw material propyl carbinol is flowed through the adsorption column of sorbent material is housed with 60-120mL/min speed;
(2) the propyl carbinol drying post after absorption is dried, and measures water content, qualified water divide be controlled at≤0.05%;
(3) water content after dry is carried out to rectifying at the propyl carbinol of acceptability limit, 180 ~ 300 DEG C of temperature at the bottom of rectifying still, 120 DEG C ~ 150 DEG C of propyl carbinol fluid temperatures in still, 116 DEG C ~ 118 DEG C of still top temperature, control reflux ratio 10:3 ~ 8;
(4) rectifying liquid after filtration, obtains high-purity organic solvent propyl carbinol product.
And, the high 1.2M of adsorption column in described step (1), diameter 3.8cm, is equipped with respectively silica gel, diatomite 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 described dry post is anhydrous magnesium sulfate or Anhydrous potassium carbonate.
Advantage of the present invention and positively effect are:
1, be about 99.5% propyl carbinol taking content be raw material to this purification process, carries out fractionation by adsorption using silica gel, diatomite 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 through absorption, dry, rectifying purifying the propyl carbinol product that purity is greater than 99.9%, this purification process is simple, and product purity is high, stable, can be used for large-scale production.
2, silica gel for this purification process, diatomite as sorbent material adsorb, anhydrous magnesium sulfate or Anhydrous potassium carbonate dry, can promote propyl carbinol content to being greater than 99.9%, all other indexs can 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, be more suitable for large-scale production and application, there is significant economic benefit.
3, the product that this purification process is produced after testing its indices meets the requirement of high-purity organic solvent propyl carbinol, its propyl carbinol content is greater than 99.9%, the rate of recovery is greater than 92%, and yield rate reaches 92%, can meet the client who uses high-purity organic solvent propyl carbinol in the demand of the aspects such as scientific experiment.
Specific embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A purification process for high-purity organic solvent propyl carbinol, step is as follows:
(1) raw material propyl carbinol (content is about 99.5%) is promoted to adsorption column top, propyl carbinol raw material adsorbs with 60mL/min speed; The wherein high 1.2M of adsorption column, diameter 3.8cm, is equipped with respectively silica gel, diatomite in two posts, its particle diameter is respectively 0.5 ~ 1.0mm and 0.3mm ~ 0.8mm, two posts series connection, 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, after fluid inspection upon adsorption approaches qualified (concrete technical requirement is in table 1), enters next-step operation, and removes absorption front-end volatiles.
(2) propyl carbinol above-mentioned adsorption column being flowed out enters dry post, the high 1.2M of post, and diameter 3.8cm, packs into through toasting dry anhydrous magnesium sulfate, detects the water content of dry rear propyl carbinol, and moisture controlled is ≤0.05%.If when moisture content is greater than 0.1%, need to carry out again drying treatment after replacing siccative.
(3) above-mentioned propyl carbinol is after drying flow to rectifying still and carry out rectifying, for further dry, in still, add the amount of hydrolith to be about 0.3% of propyl carbinol quality; Utilize electrically heated, approximately 180 DEG C of temperature at the bottom of control rectifying still, approximately 120 DEG C of propyl carbinol fluid temperatures in still, 116 DEG C ± 1 DEG C of still top temperature, controls reflux ratio 10:3 ~ 5 fluid.
(4) finished product is after 0.45 μ m filtering with microporous membrane, and under nitrogen protection, bottling sealing, obtains qualified high-purity organic solvent propyl carbinol product (purity is greater than 99.9%), and its front-end volatiles are processed in addition.
Embodiment 2:
A purification process for high-purity organic solvent propyl carbinol, step is as follows:
(1) raw material propyl carbinol (content is about 99.5%) is promoted to adsorption column top, propyl carbinol raw material adsorbs with 120mL/min speed; The wherein high 1.2M of adsorption column, diameter 3.8cm, is equipped with respectively silica gel, diatomite in two posts, its particle diameter is respectively 0.5～1.0mm and 0.3mm ~ 0.8mm, two posts series connection, 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, after fluid inspection upon adsorption approaches qualified (concrete technical requirement is in table 1), enters next-step operation, and removes absorption front-end volatiles.
(2) propyl carbinol above-mentioned adsorption column being flowed out enters dry post, the high 1.2M of post, diameter 3.8cm, pack into through toasting dry Anhydrous potassium carbonate, detect the water content of dry rear propyl carbinol, moisture controlled ,≤0.05%, if when moisture content is greater than 0.1%, needs to carry out drying treatment after replacing siccative again.
(3) above-mentioned propyl carbinol is after drying flow to rectifying still and carry out rectifying, for further dry, in still, add the amount of hydrolith to be about 0.3% of propyl carbinol quality.Utilize electrically heated, approximately 300 DEG C of temperature at the bottom of control rectifying still, approximately 150 DEG C of propyl carbinol fluid temperatures in still, 118 DEG C ± 1 DEG C of still top temperature, controls reflux ratio 10:6 ~ 8 fluid.
(4) finished product is after 0.45 μ m filtering with microporous membrane, and under nitrogen protection, bottling sealing, obtains qualified high-purity organic solvent propyl carbinol product (purity is greater than 99.9%), and its front-end volatiles are processed in addition.
Effect detection:
Purified high-purity organic solvent propyl carbinol, (1cm quartz cuvette within the scope of ultraviolet wavelength 210nm ~ 400nm, water is made reference), absorbancy meets the index request in table 1, and content is greater than 99.9%, moisture≤0.05%, the rate of recovery is greater than 92%, yield rate approximately reaches more than 92%, and all other all meet desired value, can meet 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 (1)
1. a purification process for high-purity organic solvent propyl carbinol, is characterized in that: the step of purification process is as follows:
(1) raw material propyl carbinol is flowed through the adsorption column of sorbent material is housed with 60-120mL/min speed;
(2) the propyl carbinol drying post after absorption is dried, and measures water content, qualified water divide be controlled at≤0.05%;
(3) water content after dry is carried out to rectifying at the propyl carbinol of acceptability limit, 180～300 DEG C of temperature at the bottom of rectifying still, 120 DEG C～150 DEG C of propyl carbinol fluid temperatures in still, 116 DEG C～118 DEG C of still top temperature, control reflux ratio 10:3～8;
(4) rectifying liquid after filtration, obtains the organic solvent propyl carbinol product that content is greater than 99.9%;
The adsorption column high 1.2m of described step in (1), diameter 3.8cm, is equipped with respectively silica gel, diatomite 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; Siccative in described dry post is anhydrous magnesium sulfate or Anhydrous potassium carbonate.
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| 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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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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