CN102060650A - Method for purifying chromatographic grade toluene - Google Patents
Method for purifying chromatographic grade toluene Download PDFInfo
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- CN102060650A CN102060650A CN2010106119571A CN201010611957A CN102060650A CN 102060650 A CN102060650 A CN 102060650A CN 2010106119571 A CN2010106119571 A CN 2010106119571A CN 201010611957 A CN201010611957 A CN 201010611957A CN 102060650 A CN102060650 A CN 102060650A
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- toluene
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- grade toluene
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Abstract
The invention relates to a method for purifying chromatographic grade toluene, comprising the following steps: using adsorbents to absorb and remove impurities such as a small quantity of benzene, xylene, alkane, tracethiophene and the like; dewatering with a drying agent; and rectifying according to the production process setting conditions so as to further remove the impurities in the toluene; finally, and obtaining the chromatographic grade toluene. In the purifying technology steps, alumina and celaton are used as the adsorbents to remove inorganic impurities in a raw material, anhydrous potassium carbonate or calcium sulfate is taken as the drying agent for dewatering, and finally rectification is carried out based on the process setting conditions to obtain the chromatographic grade toluene with more than 99.8% of purity, wherein the yield is larger than 95%. The purification method is simple in technology process and is convenient for operation; and compared with the conventional purification method, the purification method has the advantages of high-purity product, stable operation and the like, and is suitable for large-scale production.
Description
Technical field
The invention belongs to the chemical reagent field, relate to the purification process of high-purity chromatographic grade special agent, especially a kind of preparation method of chromatographic grade toluene.
Background technology
Toluene mainly is the aromizing acquisition by the fractionation of coal tar or oil.Therefore, wherein be mixed with many impurity, though methylbenzene raw material be purified to 〉=99%, but still have small amount of impurities, can not satisfy high-tech research and experimental requirements; And, domestic purification process to high-purity chromatorgaphy reagent is because of the reason of technical know-how, seldom report, though this product of minority manufacturer production is arranged, but quality level differs greatly, and very unstable in the application, most R﹠D institutions also depend on import, as seen China lags behind the develop rapidly of current scientific research to the development of high-purity chromatorgaphy reagent, and the purification process of research chromatographic grade reagent toluene is significant.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art level, a kind of purification process of chromatographic grade toluene is provided, present method can effectively be removed impurity such as a spot of benzene, dimethylbenzene, alkane and micro-thiophene in the toluene, prepares the chromatographic grade toluene that satisfies high-purity chromatorgaphy reagent.
The objective of the invention is to be achieved through the following technical solutions:
A kind of purification process of chromatographic grade toluene, the step of purifying is as follows:
(1) absorption: methylbenzene raw material liquid is squeezed into the adsorption column that aluminum oxide is housed,, make it with 50～100mL/min flow velocity, two adsorption columns of flowing through successively again by diatomaceous adsorption column is housed;
(2) drying: the toluene after will adsorbing is flowed through the dry post of siccative is housed, and toluene is flowed through with 50～100mL/min flow velocity the dry post of siccative is housed, and the water content of dry back toluene is controlled at≤and 0.03%;
(3) rectifying: dried toluene is squeezed into rectifying still, 150 ℃～200 ℃ of control rectifying still Heating temperatures, liquid is 120 ℃～150 ℃ in the still, 110 ℃～111 ℃ of still top temperature, total reflux 1.0h～3.0h sets reflux ratio 1: 0.5～9, removes front-end volatiles, the rectifying fluid meets solution filtering with microporous membrane after the index, and filtrate is chromatographic grade toluene product.
And the purity of described methylbenzene raw material is 99.1%～99.5%.
And described sorbent material is that aluminum oxide grain size is 100 orders～200 orders, or the diatomite granularity is 20 orders～60 orders.
And described siccative is Anhydrous potassium carbonate or calcium sulfate.
And the Intake Quantity of described siccative is 4/5 of a dry column length.
And the specification of described dry post is identical with adsorption column.
Advantage of the present invention and positively effect are:
1, the present invention is a raw material with the toluene of content about 〉=99%, through adsorbents adsorb, siccative drying, rectifying, obtain purity greater than 99.8% chromatographic grade toluene, product yield is greater than 95%, and wherein every technical indicator all reaches the requirement (technical indicator sees Table 1) of chromatographic grade toluene.
2, purifying process step of the present invention is that sorbent material is removed impurity such as a spot of benzene, dimethylbenzene, alkane and micro-thiophene, used desiccant dehydration again for adopting aluminum oxide and diatomite, presses the rectifying of technique initialization condition at last, promptly obtains qualified product.This preparation process is simple, compare with existing method have the product purity height, stable, the easy to operate and advantage that is suitable for large-scale production.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1:
A kind of purification process of chromatographic grade toluene, its step is as follows:
(1) absorption: methylbenzene raw material liquid is squeezed into adsorption column, absorption column length 1.2m, interior through 3.0cm, wherein the dress granularity is 100 orders～200 purpose aluminum oxide in one, another root dress granularity 20 orders～60 purpose diatomite, toluene carries out adsorption-edulcoration with 50mL/min flow velocity two adsorption columns of successively flowing through;
This step fully contacts absorption by aluminum oxide, diatomite with toluene, to remove wherein a spot of organic class impurity.
(2) drying: the toluene after will adsorbing is flowed through the dry post of siccative Anhydrous potassium carbonate is housed, the same adsorption column of the specification of pillar, the amount of dress siccative is 4/5 of a column length, and toluene carries out drying with the 50mL/min flow velocity dry post of flowing through, dry back toluene water content is controlled at≤and 0.03%;
Utilize siccative such as Anhydrous potassium carbonate to remove the moisture in the toluene after adsorbing in this step,, proceed drying treatment again after then need changing siccative as moisture content＞0.05% o'clock.
(3) rectifying: dried toluene is squeezed into rectifying still, utilize electrically heated, 150 ℃～200 ℃ of control rectifying still Heating temperatures, liquid is 120 ℃～150 ℃ in the still, 110 ℃～111 ℃ of still top temperature.Total reflux 1.0h～1.5h sets reflux ratio 1: 0.5～4, removes front-end volatiles, after the rectifying fluid meets index, with 0.45 μ m filtering with microporous membrane, adorns brown reagent bottle, and inflated with nitrogen is preserved, and promptly gets the chromatographic grade toluene product that meets index request.
Embodiment 2:
A kind of preparation method of chromatographic grade toluene, its step is as follows:
(1) absorption: methylbenzene raw material liquid is squeezed into adsorption column, absorption column length 1.2m, interior through 3.0cm, wherein the dress granularity is 100 orders～200 purpose aluminum oxide in one, another root dress granularity 20 orders～60 purpose diatomite, toluene carries out adsorption-edulcoration with 100mL/min flow velocity two adsorption columns of successively flowing through;
This step fully contacts absorption with diatomite with toluene by the sorbent material aluminum oxide, to remove wherein a spot of organic class impurity.
(2) drying: the toluene after will adsorbing is flowed through the dry post of siccative calcium sulfate is housed, the same adsorption column of the specification of pillar, the amount of dress siccative is 4/5 of a column length, toluene is with the 100mL/min flow velocity dry post of flowing through, carry out drying, dry back water content is controlled at≤and 0.03%;
(3) rectifying: dried toluene is squeezed into rectifying still, utilize electrically heated, 150 ℃～200 ℃ of control rectifying still Heating temperatures, liquid is about 120 ℃～150 ℃ in the still, about 110 ℃～111 ℃ of still top temperature.Total reflux 1.5h～3.0h, set reflux ratio 1: 5～9 (all being presented on the instrument controlling box), remove front-end volatiles (handling in addition), after the rectifying fluid meets index, with 0.45 μ m filtering with microporous membrane, adorn brown reagent bottle, inflated with nitrogen is preserved, and promptly gets the chromatographic grade toluene product that meets index request.
Effect detection:
Chromatogram organic solvent toluene behind the purifying is in ultraviolet wavelength 285nm～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 99.8%, moisture≤0.03%, the rate of recovery is greater than 95%, and all other satisfy chromatographic grade index request.
Table 1 chromatographic grade toluene technical indicator
Claims (6)
1. the purification process of a chromatographic grade toluene, it is characterized in that: the step of purifying is as follows:
(1) absorption: methylbenzene raw material liquid is squeezed into the adsorption column that aluminum oxide is housed,, make it with 50～100mL/min flow velocity, two adsorption columns of flowing through successively again by diatomaceous adsorption column is housed;
(2) drying: the toluene after will adsorbing is flowed through the dry post of siccative is housed, and toluene is flowed through with 50～100mL/min flow velocity the dry post of siccative is housed, and the water content of dry back toluene is controlled at≤and 0.03%;
(3) rectifying: dried toluene is squeezed into rectifying still, 150 ℃～200 ℃ of control rectifying still Heating temperatures, liquid is 120 ℃～150 ℃ in the still, 110 ℃～111 ℃ of still top temperature, total reflux 1.0h～3.0h sets reflux ratio 1: 0.5～9, removes front-end volatiles, the rectifying fluid meets solution filtering with microporous membrane after the index, and filtrate is chromatographic grade toluene product.
2. the purification process of chromatographic grade toluene according to claim 1 is characterized in that: the purity of described methylbenzene raw material is 99.1%～99.5%.
3. the purification process of chromatographic grade toluene according to claim 1 is characterized in that: described sorbent material is that aluminum oxide grain size is 100 orders～200 orders, or the diatomite granularity is 20 orders～60 orders.
4. the purification process of chromatographic grade toluene according to claim 1 is characterized in that: described siccative is Anhydrous potassium carbonate or calcium sulfate.
5. according to the purification process of claim 1 or 4 described chromatographic grade toluene, it is characterized in that: the Intake Quantity of described siccative is 4/5 of a dry column length.
6. the purification process of chromatographic grade toluene according to claim 1 is characterized in that: the specification of described dry post is identical with adsorption column.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010106119571A CN102060650A (en) | 2010-12-29 | 2010-12-29 | Method for purifying chromatographic grade toluene |
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| CN2010106119571A CN102060650A (en) | 2010-12-29 | 2010-12-29 | Method for purifying chromatographic grade toluene |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964200A (en) * | 2012-11-26 | 2013-03-13 | 北京旭阳化工技术研究院有限公司 | Purifying method of coking toluene |
| CN104692996A (en) * | 2013-12-05 | 2015-06-10 | 华东师范大学 | Method for removing nitrate ions in toluene by using diatomite |
| CN107501030A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatogram pure toluene and preparation method thereof, production system |
| CN107915567A (en) * | 2016-10-08 | 2018-04-17 | 中国石油化工股份有限公司 | The method that polar compound is removed from the aromatic raw material containing polar compound |
| CN112585106A (en) * | 2018-08-10 | 2021-03-30 | 环球油品有限责任公司 | Process for producing high-purity p-xylene and high-purity toluene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106370A (en) * | 1994-10-22 | 1995-08-09 | 中国石化扬子石油化工公司 | Improved method for producing high pure para-xylene through adsorption separation |
| 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 |
-
2010
- 2010-12-29 CN CN2010106119571A patent/CN102060650A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106370A (en) * | 1994-10-22 | 1995-08-09 | 中国石化扬子石油化工公司 | Improved method for producing high pure para-xylene through adsorption separation |
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964200A (en) * | 2012-11-26 | 2013-03-13 | 北京旭阳化工技术研究院有限公司 | Purifying method of coking toluene |
| CN102964200B (en) * | 2012-11-26 | 2014-09-17 | 北京旭阳化工技术研究院有限公司 | Purifying method of coking toluene |
| CN104692996A (en) * | 2013-12-05 | 2015-06-10 | 华东师范大学 | Method for removing nitrate ions in toluene by using diatomite |
| CN107915567A (en) * | 2016-10-08 | 2018-04-17 | 中国石油化工股份有限公司 | The method that polar compound is removed from the aromatic raw material containing polar compound |
| CN107501030A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatogram pure toluene and preparation method thereof, production system |
| CN112585106A (en) * | 2018-08-10 | 2021-03-30 | 环球油品有限责任公司 | Process for producing high-purity p-xylene and high-purity toluene |
| CN112585106B (en) * | 2018-08-10 | 2023-09-08 | 环球油品有限责任公司 | Method for producing high-purity para-xylene and high-purity toluene |
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Application publication date: 20110518 |