CN102126913B - Method for separating indan and tetraline through composite extractive distillation - Google Patents
Method for separating indan and tetraline through composite extractive distillation Download PDFInfo
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- CN102126913B CN102126913B CN 201010579319 CN201010579319A CN102126913B CN 102126913 B CN102126913 B CN 102126913B CN 201010579319 CN201010579319 CN 201010579319 CN 201010579319 A CN201010579319 A CN 201010579319A CN 102126913 B CN102126913 B CN 102126913B
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Abstract
The invention discloses a method for separating indan and tetraline through composite extractive distillation. The method comprises the following steps: (1) the composite solvent consisting of sulfolane and N-formylmorpholine and the raw material liquid containing indan and tetraline enter an extractive distillation column according to a certain solvent ratio, wherein the number of theoretical plates is 50-55, the reflux ratio is (2.5-4):1, the tower top temperature is 90-95 DEG C, the feeding temperature of the composite solvent is 80-85 DEG C, more than 99.0wt% of indan product is obtained from the tower top and the mixed fraction of the composite solvent and tetraline is in the tower bottom; and (2) the mixed fraction in the tower bottom enters from the middle of a solvent recycling tower, wherein the number of theoretical plates is 20-25, the reflux ratio is 2.5-4.0, the tower top temperature is 120-125 DEG C, more than 99.0wt% of tetraline product is obtained from the tower top, and the composite solvent recycled from the tower bottom returns to the extractive distillation column to be recycled. Compared with the common distillation process, in the composite extractive distillation process in the invention, the separation efficiency is greatly increased and the equipment investment and energy consumption can be obviously reduced. Therefore, the composite extractive distillation process is an efficient and energy-saving separation process.
Description
Technical field
The invention belongs to the processing method of chemical separation process, relate to a kind of method that adopts the double solvents extracting rectifying to separate indane and tetraline.
Background technology
Coal tar is the bulk product of coking chemical, contains up to ten thousand kinds of organic compound approximately, can identify about 500 at present surplus kind, wherein coking crude benzene is the byproduct of coal tarization, is an important channel that obtains purified petroleum benzin at present.China's coking crude benzene output was about 4,800,000 tons in 2009, hydrogenation liquid the heavy component raffinate through remove BTX (benzene,toluene,xylene) after of coking crude benzene after by hydrogenation reaction contains many important organic compound, wherein indane accounts for 25%, tetraline accounts for 30%, these compounds all are the precious resources of development fine chemistry industry, have very high economic worth.
Indane has another name called 2,3-dihydro indenes, colourless liquid, and boiling point is 176.5 ℃, can be used as shockproof dose of shockproof dose of aviation fuel, rubber industry etc., also can be used as raw material and the solvent of organic synthesis simultaneously.Tetraline is colourless liquid, and boiling point is 207.4 ℃, in a large number for the production of fields such as Wimet forming agent, paint, medicine intermediate and papermaking.Although the boiling point of the boiling point of indane and tetraline differs near 30 ℃, because special phase equilibrium relationship between indane and the tetraline, for example the relative volatility α of indane and tetraline=1.05 when normal pressure belong to the extremely difficult system that separates.By the conventional distillation of routine to obtain to satisfy market demands indane (〉=99.0wt%) and the tetraline product (〉=99.0wt%), then the theoretical plate number of rectifying tower need be above 150, and reflux ratio surpasses 20, so the energy consumption of process and facility investment are all bigger, see Fig. 1.
In view of the difficult present situation of separating of indane and tetraline, as if developing methods such as extracting rectifying in a kind of separating technology efficiently such as the special extract rectification or azeotropic distillation, will have high economic benefit and social benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method that adopts composite extraction and rectification to separate indane and tetraline is provided, the double solvents that utilizes tetramethylene sulfone and N-N-formyl morpholine N-to form with certain proportioning, mixed solution to indane and tetraline carries out extracting rectifying, thereby increase relative volatility between the two, make it more easily realize separating, thereby obtain high purity indane and tetraline product, double solvents can be recycled behind solvent recovery tower simultaneously.
Present method is compared with the conventional distillation separation method, has improved separation efficiency greatly, has significantly reduced facility investment and process energy consumption, is a kind of energy-efficient separating technology.
The invention provides the separating technology of a kind of double solvents extracting rectifying indane and tetraline, comprise abstraction distillation system and solvent recovering system.The concrete steps of finishing technology of the present invention are as follows:
(1) extracting rectifying process: indane and tetraline raw mix add from the extractive distillation column middle part, double solvents according to certain solvent ratio adds from extractive distillation column top in specified for temperature ranges through heat exchange, overhead vapours behind condenser necessarily the reflux ratio extraction obtain the indane product, the mixing solutions that is rich in double solvents and tetraline enters solvent recovery tower;
(2) solvent recuperation process: the mixing solutions that is rich in double solvents and tetraline enters the solvent recovery tower middle part, and cat head is with certain reflux ratio extraction tetraline, and the double solvents that reclaims at the bottom of the tower is back to extractive distillation column and recycles after reclaiming.
Double solvents of the present invention refers to that main solvent is tetramethylene sulfone, and solubility promoter is the N-N-formyl morpholine N-, and both quality proportionings are 80～85: 20～15, optimal proportion 85: 15.
Invent described " solvent ratio " and refer to the volume ratio of circulation double solvents and indane and the tetraline raw mix of extractive distillation column, this solvent ratio is 3.5～5: 1, and optimum solvent than 4 is: 1.
In step (1), the number of theoretical plate of described extractive distillation column is preferably 50～55, and the cat head working pressure is preferably 10～12.0kPa, more preferably 10kPa, solvent ratio is 3.5～5: 1, reflux ratio is 2～3: 1, and tower top temperature was preferably 90～95 ℃ in more preferably 4: 1, more preferably 90 ℃, the tower reactor temperature is preferably 145～165 ℃, more preferably 145 ℃, the composite extractant inlet temperature of stabilizer is 80～85 ℃, more preferably 85 ℃.
In step (2), the number of theoretical plate of described solvent recovery tower is preferably 20～25, the cat head working pressure is preferably 8～10kPa, 10kPa more preferably, reflux ratio is 0.5～1: 1, more preferably 1: 1, tower top temperature is preferably 120～125 ℃, more preferably 120 ℃, the tower reactor temperature is preferably 180～190 ℃, more preferably 180 ℃.
The method that double solvents extracting rectifying of the present invention separates indane and tetraline has following characteristics:
(1) separate indane with the conventional distillation process and compare with tetraline, the extractive distillation column number of theoretical plate of extraction rectification technique reduces significantly, and this facility investment reduces more;
(2) operating reflux ratio of double solvents extracting rectifying process reduces significantly, and novel process considered the hot integrated of internal process logistics, so extracting rectifying process energy consumption is lower;
(3) the double solvents extracting rectifying separation process scheme of indane and tetraline is simple, process automation degree height, and the indane that obtains and tetraline good product quality have favorable economic benefit and social benefit.
Description of drawings
Fig. 1 is the conventional distillation separation process scheme figure of indane and tetraline, and Fig. 2 is the double solvents extracting rectifying separation process scheme figure of indane and tetraline.
The 1-double solvents; The 2-stock liquid; 3-solvent interchanger; The 4-extractive distillation column; 5-extractive distillation column condenser; 6-indane product; 7-extractive distillation column reboiler; The double solvents that 8-replenishes; 9-extracting rectifying tower reactor liquid; The 10-solvent recovery tower; 11-solvent recovery tower condenser; 12-tetraline product; 13-solvent recovery tower reboiler; 14-solvent recuperation tower reactor liquid (circulation double solvents).
Embodiment
Below in conjunction with embodiment, further specify the present invention, but the present invention is not limited to embodiment.
The heavy component raffinate of certain enterprise's coking crude benzene hydrogenation liquid after removing BTX, the indane and the tetraline raw material mixed solution composition that obtain by further Separation and Recovery see Table 1.
Table 1 indane and tetraline stock liquid are formed
| Component | Form (wt%) |
| Indane | 45 |
| Tetraline | 55 |
Indane and tetraline stock liquid 2 are that 1000kg/hr enters extractive distillation column 4 middle parts with the flow, double solvents 1 ℃ enters extractive distillation column top according to 4: 1 volume ratio through interchanger 3 heat exchange to 85, the quality proportioning of tetramethylene sulfone and N-N-formyl morpholine N-is 85: 15 in the double solvents, this tower number of theoretical plate is 55, tower top pressure is 10.0kPa, tower top temperature is 90 ℃, the tower reactor temperature is 145 ℃, tower bottom irregularly replenishes 2.0kg/hr double solvents 8 simultaneously, overhead vapours is the indane 6 that 3: 1 extraction product purities are 99.4wt% with reflux ratio after condenser 5 condensations, double solvents at the bottom of the tower and tetraline mixed solution 9 enter solvent recovery tower 10 middle parts, this tower number of theoretical plate is 20, tower top pressure is 10kPa, reflux ratio is 1: 1, tower top temperature is 125 ℃, the tower reactor temperature is 190 ℃, overhead vapours is that 1: 1 extraction product purity is the tetraline product 12 more than the 99.6wt% with reflux ratio after condenser 11 condensations, and the double solvents that solvent recuperation tower reactor liquid 14 is regeneration can be recycled.
In this process, the thermal load that extractive distillation column reboiler 7 and solvent recovery tower reboiler 13 consume is total up to 0.85MCAL/hr, and the middle pressure steam consumption is total up to 2.25t/h; The refrigeration duty of interchanger 3, condenser 5 and condenser 7 is total up to 0.87MCAL/hr, and cooling water consumption is total up to 315t/hr.
Comparative Examples
Indane and tetraline stock liquid composition see Table 1, carry out the conventional distillation operation, inlet amount is 1000kg/h, and theoretical number of plates of rectifying tower is 150, and reflux ratio is 24: 1, working pressure is 10kPa, tower top temperature is 90 ℃, and the tower reactor temperature is 130.0 ℃, obtains the indane product of 99.1wt% at cat head, tower reactor obtains 99.2% tetraline product, and stock liquid charging simultaneously and tower reactor cut carry out abundant heat exchange to utilize internal heat.The thermal load of rectifying tower reboiler is 1.21MCAL/hr, and the middle pressure steam consumption is 3.12t/h; The refrigeration duty of overhead condenser is 1.20MCAL/hr, and cooling water consumption is 440t/h.Extraction rectification technique is compared with conventional distillation technology, and the middle pressure steam consumption has saved 27.9%, and cooling water consumption saves 28.4%, and obviously higher the and energy consumption of the double solvents extraction rectification technique separation efficiency that adopts reduces greatly.
Claims (4)
1. method that adopts the double solvents extracting rectifying to separate indane and tetraline, it is characterized in that double solvents (1) is made up of main solvent and solubility promoter, main solvent is tetramethylene sulfone, and solubility promoter is the N-N-formyl morpholine N-, and the quality proportioning of main solvent and solubility promoter is 80～85: 20～15;
1) double solvents (1) enters in the tower from extractive distillation column (4) middle and upper part by certain solvent ratio with the stock liquid (2) of indane and tetraline and separates, cat head obtains the above indane product (6) of 99.0wt%, obtains containing the mixed fraction (9) of double solvents and tetraline at the bottom of the tower;
2) tower reactor mixed fraction (9) is discharged at the bottom of the extractive distillation column and is entered the solvent recovery tower middle part, and cat head obtains the tetraline product (12) 99.0% or more, tower reactor for regeneration after double solvents (13), return to extractive distillation column and recycle.
2. according to a kind of method that adopts the double solvents extracting rectifying to separate indane and tetraline of claim 1, it is characterized in that double solvents (1) and the volume ratio of stock liquid are 3.5～5: 1.
3. method according to claim 1, the operational condition that it is characterized in that extractive distillation column is: number of theoretical plate is 50～55, tower top pressure is 10～12.0kPa, double solvents (1) is 3.5～5: 1 with the volume ratio of stock liquid, reflux ratio is 2～3: 1, tower top temperature is 90～95 ℃, and the tower reactor temperature is 145～165 ℃, and double solvents (1) inlet temperature of stabilizer is 80～85 ℃.
4. method according to claim 1, it is characterized in that the operational condition of solvent recovery tower is: number of theoretical plate is 20～25, and tower top pressure is 8～10kPa, and reflux ratio is 0.5～1: 1, and tower top temperature is 120～125 ℃, the tower reactor temperature is 180～190 ℃.
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| CN 201010579319 CN102126913B (en) | 2010-12-03 | 2010-12-03 | Method for separating indan and tetraline through composite extractive distillation |
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| CN102126913B true CN102126913B (en) | 2013-07-10 |
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| CN104876787B (en) * | 2015-06-12 | 2017-01-04 | 云南大为恒远化工有限公司 | A kind of method purifying tetrahydronaphthalene from coking crude benzene hydrogenation liquid |
| CN112457879A (en) * | 2020-11-12 | 2021-03-09 | 河北中化鑫宝化工科技有限公司 | Method and device for extracting high-purity indene from coal tar indene fraction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3210259A (en) * | 1961-06-26 | 1965-10-05 | Monsanto Co | Extractive separation process |
| US4053369A (en) * | 1974-05-30 | 1977-10-11 | Phillips Petroleum Company | Extractive distillation |
| CN1091413A (en) * | 1992-11-17 | 1994-08-31 | 克鲁普科普斯有限公司 | Method with seperation of hydrocarbon mixture as function of extractive distillation |
| US6005157A (en) * | 1998-05-11 | 1999-12-21 | Hfm International, Inc. | Cycloparaffin purification from petroleum streams |
-
2010
- 2010-12-03 CN CN 201010579319 patent/CN102126913B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3210259A (en) * | 1961-06-26 | 1965-10-05 | Monsanto Co | Extractive separation process |
| US4053369A (en) * | 1974-05-30 | 1977-10-11 | Phillips Petroleum Company | Extractive distillation |
| CN1091413A (en) * | 1992-11-17 | 1994-08-31 | 克鲁普科普斯有限公司 | Method with seperation of hydrocarbon mixture as function of extractive distillation |
| US6005157A (en) * | 1998-05-11 | 1999-12-21 | Hfm International, Inc. | Cycloparaffin purification from petroleum streams |
Non-Patent Citations (4)
| Title |
|---|
| Claudia Irina KONCSAG et al.The characterization by chromatographic methods of petroleum fractions from thermocatalytical processes.《Ovidius University Annals of Chemistry 》.2009,第20卷(第1期),第5-10页. |
| The characterization by chromatographic methods of petroleum fractions from thermocatalytical processes;Claudia Irina KONCSAG et al;《Ovidius University Annals of Chemistry 》;20091231;第20卷(第1期);第5-10页 * |
| 王萍等.重烷苯中二烷基苯和茚满萘满的分离与鉴定.《日用化学工业》.2005,第35卷(第2期),第119-122页. |
| 重烷苯中二烷基苯和茚满萘满的分离与鉴定;王萍等;《日用化学工业》;20050430;第35卷(第2期);第119-122页 * |
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