CN101575261A - Method for extracting, rectifying and separating pseudocumene and indane - Google Patents
Method for extracting, rectifying and separating pseudocumene and indane Download PDFInfo
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- CN101575261A CN101575261A CNA2009100332453A CN200910033245A CN101575261A CN 101575261 A CN101575261 A CN 101575261A CN A2009100332453 A CNA2009100332453 A CN A2009100332453A CN 200910033245 A CN200910033245 A CN 200910033245A CN 101575261 A CN101575261 A CN 101575261A
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Abstract
The invention discloses a method for extracting, rectifying and separating pseudocumene and indane, which comprises the following steps: (1) using sulfolane as a solvent for extractive rectification, and adding the sulfolane and a raw material mixture into an extractive rectification tower according to a certain proportion; (2) after separation, leaving the high-purity pseudocumene at the tower top, and leaving the sulfolane solvent and the indane at the tower bottom; (3) delivering the tower bottom material into a solvent regeneration tower to carry out distillation operation, wherein an extract at the tower top is the indane, and the tower bottom is the sulfolane solvent; and (4) delivering the solvent sulfolane at the tower bottom back to the extractive rectification tower for recycling. A product of the method is the pseudocumene of which the purity is more than or equal to 99.5 percent; and the extracted and rectified sulfolane solvent can be recycled, and simultaneously the reclaiming rate of the indane is more than or equal to 97 percent. Compared with the conventional common distillation method, the purity of the product is higher, the reclaiming rate is higher, and the energy consumption is lower.
Description
Technical field
The present invention relates to a kind of separation method of chemical industry, the extraction and rectification separation method of particularly a kind of unsym-trimethyl benzene and indane.
Background technology
Unsym-trimethyl benzene and indane all are important basic Organic Chemicals and organic chemical industry's solvents, indane is a raw material of making synthetic resins, unsym-trimethyl benzene is widely used in Chemical Manufacture, can be used for preparing VITAMIN, dimethylbenzene, trimellitic acid 1,2-anhydride, sym-trimethylbenzene, durol and pyromellitic acid anhydride etc., the two all is present in the by product-cracking heavy aromatics of ethylene production, it is about 5% wherein to contain unsym-trimethyl benzene, indane 1～2%.Because the existence of indane is totally unfavorable to catalyzer in the trimethylbenzene subsequent reactions, so need be with the two thorough separation.
Because unsym-trimethyl benzene boiling point (168.0 ℃) and indane boiling point (176.0 ℃) are approaching, as if with the conventional distillation method to its further separation and purification, then energy consumption is too big, has directly influenced the further development and use of this part resource.With 2008 was example, China's cracking heavy aromatics annual production is about 3,000,000 tons, if wherein unsym-trimethyl benzene separates purification with indane, can produce 150000 tons of unsym-trimethyl benzenes, about 30,000 tons of indanes per year, resource is fully used, also can increases the business economic benefit greatly.
Summary of the invention
The extraction and rectification separation method that the purpose of this invention is to provide a kind of unsym-trimethyl benzene and indane, this method is raw material (containing 80% unsym-trimethyl benzene, 20% indane) with industrial unsym-trimethyl benzene and indane mixture, with the tetramethylene sulfone is solvent, carry out the extracting rectifying operation, separate the purification unsym-trimethyl benzene, reclaim indane simultaneously, solvent sulfolane can be recycled through regeneration.Present method is compared with the common distillating method that routine is used, and product purity is higher, and the rate of recovery is higher, and energy consumption is lower.
The technical scheme of finishing the foregoing invention task is: the extraction and rectification separation method of a kind of unsym-trimethyl benzene and indane, it is characterized in that step is as follows,
(1). with the tetramethylene sulfone is the solvent of extracting rectifying, and itself and raw mix are added extractive distillation column with certain proportioning;
(2). after the separation, cat head is high purity unsym-trimethyl benzene (〉=99.5%), and the tower still is solvent sulfolane+indane;
(3). tower still material is sent into solvent regeneration tower and is carried out distillation procedure, and the cat head production is indane (〉=98%), and the tower still is a solvent sulfolane;
(4). the indane of cat head extraction can be directly as the synthetic resins raw material; Tower still solvent sulfolane can be sent extractive distillation column back to and be recycled.
" certain proportioning " of solvent of the present invention and raw mix is meant: the mass ratio of solvent and raw mix is 2/1-4/1, and best proportion is 3/1.
The technical process of sepn process is seen shown in Figure 1, and separating apparatus adopts optimizes processing condition, can obtain the high purity unsym-trimethyl benzene after the separation, simultaneously the indane rate of recovery 〉=97%.
Advantage of the present invention: adopt technical process shown in Figure 1 and optimized parameters, raw material is that industrial unsym-trimethyl benzene and indane mixture (contain 80% unsym-trimethyl benzene, 20% indane), with the tetramethylene sulfone is solvent, at first carry out the extracting rectifying operation through extractive distillation column T1, overhead product is the unsym-trimethyl benzene of purity 〉=99.5%, tower kettle product distills processing through solvent regeneration tower T2, indane in the recyclable raw material of one side, the solvent sulfolane of extracting rectifying is recycled, operate by two towers, can obtain the unsym-trimethyl benzene product of purity 〉=99.5%, and make the indane rate of recovery 〉=97% simultaneously.Compare with the common distillating method that routine is used, product purity is higher, and the rate of recovery is higher, and energy consumption is lower.
Simultaneously, because the whole process solvent can be recycled, production cost is lower, and can not throw into question to environment.
Description of drawings
Fig. 1 is the technical process of extracting rectifying and solvent reclamation.
Embodiment
The method that embodiment 1, extracting rectifying separate unsym-trimethyl benzene and indane, with reference to processing parameter shown in technical process shown in Figure 1 and the table 1,1. raw material is raw mix, and wherein the mass content of unsym-trimethyl benzene and indane is respectively 80%, 20%, flow is 5Kg/h, 9. solvent is tetramethylene sulfone, and flow is 15Kg/h, and extractive distillation column T1 tower top temperature is 168～169 ℃, tower still temperature is 255～260 ℃, control of reflux ratio is 4～5, and cat head production 3. flow is 4Kg/h, consists of x
Unsym-trimethyl benzene=0.9962, x
Indane=0.0038, tower still discharging 4. flow is 21Kg/h, consists of x
Tetramethylene sulfone=0.9524, x
Unsym-trimethyl benzene=0.0007, x
Indane=0.0469, this part discharging is the charging of solvent regeneration tower T2 simultaneously, and solvent regeneration tower T2 tower top temperature is 176～177 ℃, and tower still temperature is about 270 ℃, and control of reflux ratio is 4～5, and cat head production 7. flow is 1Kg/h, consists of x
Unsym-trimethyl benzene=0.0151, x
Indane=0.9849, tower still discharging 9. flow is 20Kg/h, and wherein tetramethylene sulfone mass content 〉=99.7% can recycle.1,3 is condenser among the figure, and 2,4 is reboiler.1.～9. be stream burst title (table 2).
Each tower process condition of table 1
| Processing parameter | The T-1 tower | The T-2 tower |
| Theoretical plate number | 60 | 40 |
| The raw material feed entrance point | 15 | 15 |
| The solvent feed position | 40 | |
| Reflux ratio | 4-5 | 4-5 |
| Tower top temperature (℃) | 168-169 | 176-177 |
| Tower still temperature (℃) | 255-260 | 265-275 |
Burst explanation of table 2 stream
Embodiment 2, and is substantially the same manner as Example 1, but the mass ratio of solvent and raw mix is 2/1.
Claims (5)
1, the extraction and rectification separation method of a kind of unsym-trimethyl benzene and indane is characterized in that, step is as follows,
(1). with the tetramethylene sulfone is the solvent of extracting rectifying, and itself and raw mix are added extractive distillation column with certain proportioning;
(2). after the separation, cat head is the high purity unsym-trimethyl benzene, and the tower still is solvent sulfolane+indane;
(3). tower still material is sent into solvent regeneration tower and is carried out distillation procedure, and the cat head production is an indane, and the tower still is a solvent sulfolane;
(4). tower still solvent sulfolane is sent extractive distillation column back to and is recycled.
2, the extraction and rectification separation method of unsym-trimethyl benzene according to claim 1 and indane is characterized in that, " certain proportioning " of described solvent and raw mix is meant: the mass ratio of solvent and raw mix is 2/1～4/1.
3, the extraction and rectification separation method of unsym-trimethyl benzene according to claim 1 and indane is characterized in that, " certain proportioning " of described solvent and raw mix is meant: the mass ratio of solvent and raw mix is 3/1.
According to the extraction and rectification separation method of claim 1 or 2 or 3 described unsym-trimethyl benzenes and indane, it is characterized in that 4, concrete parameter is as follows:
The mass content of unsym-trimethyl benzene and indane is respectively 80%, 20% in the described raw material (1.), and flow is 5Kg/h;
Solvent (9.) is a tetramethylene sulfone, and flow is 15Kg/h;
Extractive distillation column (T1) tower top temperature is 168～169 ℃, and tower still temperature is 255～260 ℃, and control of reflux ratio is 4～5;
Cat head production (3.) flow is 4Kg/h, consists of x
Unsym-trimethyl benzene=0.9962, x
Indane=0.0038, tower still discharging (4.) flow is 21Kg/h, consists of x
Tetramethylene sulfone=0.9524, x
Unsym-trimethyl benzene=0.0007, x
Indenes Full=0.0469;
Solvent regeneration tower (T2) tower top temperature is 176～177 ℃, and tower still temperature is that control of reflux ratio is 4～5 about 270 ℃;
Cat head production (7.) flow is 1Kg/h, consists of x
Unsym-trimethyl benzene=0.0151, x
Indane=0.9849, tower still discharging (9.) flow is 20Kg/h, wherein tetramethylene sulfone mass content 〉=99.7%.
5, the extraction and rectification separation method of unsym-trimethyl benzene according to claim 4 and indane is characterized in that, described rectifying tower (T1) theoretical plate number is 60; The raw material feed entrance point is 15; The extraction solvent feed entrance point is 40; Described regenerator column (T2) theoretical plate number is 40; The raw material feed entrance point is 15.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910033245 CN101575261B (en) | 2009-06-16 | 2009-06-16 | Method for extracting, rectifying and separating pseudocumene and indane |
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| CN 200910033245 CN101575261B (en) | 2009-06-16 | 2009-06-16 | Method for extracting, rectifying and separating pseudocumene and indane |
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| CN101575261A true CN101575261A (en) | 2009-11-11 |
| CN101575261B CN101575261B (en) | 2013-04-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837394A (en) * | 2016-04-05 | 2016-08-10 | 天津大学 | Purifying method of highly-pure 1,2,3-trimethylbenzene |
| CN109627139A (en) * | 2017-10-09 | 2019-04-16 | 中国石化扬子石油化工有限公司 | Indane separation method in a kind of cracking carbon nine |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226246C (en) * | 2003-06-30 | 2005-11-09 | 南京师范大学 | Rectification and extraction crossing and combining separation process of carbon 9 arene |
| CN101077849B (en) * | 2007-06-01 | 2010-08-25 | 南京师范大学 | Extraction, distillation and separation method for m-methylethylbenzene and p-methylethylbenzene |
| CN101445421A (en) * | 2008-11-04 | 2009-06-03 | 南京师范大学 | Method for extracting mixed extractant of trimethyl benzene in cracked C*; method for measuring mixed extractant and measure equipment thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837394A (en) * | 2016-04-05 | 2016-08-10 | 天津大学 | Purifying method of highly-pure 1,2,3-trimethylbenzene |
| CN105837394B (en) * | 2016-04-05 | 2018-12-21 | 天津大学 | A kind of method of purification of high-purity 1,2,3-trimethylbenzene |
| CN109627139A (en) * | 2017-10-09 | 2019-04-16 | 中国石化扬子石油化工有限公司 | Indane separation method in a kind of cracking carbon nine |
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