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