CN100460373C - Method for extracting rectifying and separating benzene - Google Patents
Method for extracting rectifying and separating benzene Download PDFInfo
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- CN100460373C CN100460373C CNB2006100080745A CN200610008074A CN100460373C CN 100460373 C CN100460373 C CN 100460373C CN B2006100080745 A CNB2006100080745 A CN B2006100080745A CN 200610008074 A CN200610008074 A CN 200610008074A CN 100460373 C CN100460373 C CN 100460373C
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Abstract
A process for separating benzene by extracting rectifying includes such steps as adding the hydrocarbon mixture containing olefin and benzene into extracting-rectifying tower, contacting with extracting solvent for extracting rectifying, discharging the extracting solvent containing benzene from bottom, adding it into solvent recovering tower for separating benzene from solvent, discharging benzene fraction from its top, condensing, refining in argil tower, flash evaporation in flash tower, discharging the substance from its top, and condensing to obtain benzene.
Description
Technical field
The present invention is a kind of method of extracting rectifying and separating benzene, specifically, be a kind of from the hydrocarbon mixture that contains alkene the method for extracting rectifying and separating benzene.
Background technology
The method of Separation of Benzene mainly contains two classes from reformed oil and cracking hydrogenated gasoline.One class is a liquid-liquid extraction method, and another kind of is extraction fractional distillation.Liquid-liquid extraction method at present more uses moisture tetramethylene sulfone as extraction solvent, its shortcoming is the raw material that is not suitable for high aromaticity content, and the benzene that extracting and separating goes out is because of moisture its freezing point that influences, need behind clay tower, to be provided with complexity and the more benzene tower of stage number, separate water outlet in the benzene column overhead, side line obtains purified petroleum benzin, and a spot of heavy impurity is discharged at the bottom of tower.The process of this extraction separation of benzol is comparatively complicated, and equipment and process cost are all higher.Particularly,, adopt aqueous sulfolane solvent, because its dissolving power is too little and inapplicable because the content of benzene is lower in the extraction feed in the catalytic reforming field.Compare with liquid-liquid extraction process, the extracting rectifying rule have flow process and simple to operate, facility investment is low, low power consumption and other advantages.Therefore, utilize extracting rectifying to separate purified petroleum benzin in the raw material under the more situation of aromaticity content and have more advantage.
The method of existing extracting rectifying and separating benzene mostly is the flow process of extracting rectifying-solvent recuperation-product purification greatly; the benzene cut that obtains from the solvent recuperation cat head removes through carclazyte behind the alkene of trace directly as benzaldehyde product, and the extraction solvent of selecting for use mainly contains N-Methyl pyrrolidone (NMP), N-formyl morpholine (NFM) or tetramethylene sulfone.The problem that this method exists is when handling the higher raw material of olefin(e) centent, to generate oil, the benzaldehyde product quality instability that obtains as CONTINUOUS REFORMER.The alkene that contains in the extracting rectifying raw material separates with aromatic hydrocarbons than alkane is more difficult, particularly cycloolefin, diolefine and alkatrienes, as cyclopentadiene, cyclohexadiene etc., this class alkene boiling point and benzene are approaching, and structure and benzene are approximate, tend to enter benzaldehyde product in the extracting rectifying process, influence the pickling chromatic number of benzaldehyde product, therefore need the frequent carclazyte of changing.The pickling chromatic number of regulation benzene is not more than 1 in country's top grade product purified petroleum benzin quality standard, will cause the pickling chromatic number greater than 1 and contain trace amounts of olefin in the purified petroleum benzin.When the crude benzol that contains trace amounts of olefin passed through carclazyte, micromolecular olefinic polymerization was macromolecular heavy olefins under the effect of carclazyte acid sites.This heavy olefins may be two olefin hydrocarbon molecules or three olefin hydrocarbon molecules even a plurality of molecule formation, various and each component concentration of their component seldom, make the carclazyte use initial stage have certain adsorptive power, when above-mentioned heavy olefins is attracted to the carclazyte surface, very fast promptly reach absorption saturated, heavy olefins in the crude benzol will flow out with benzene, although its content is few, is enough to make the pickling chromatic number of benzaldehyde product to increase.
At present, ethylene cracker all has a pyrolysis gasoline hydrogenation device because pyrolysis gasoline alkene, foreign matter content are higher, olefin(e) centent is very low in the cracking hydrogenated gasoline that obtains, usually do not influence the quality of benzaldehyde product, and reformer is because the needs of whole flow process, and in reforming process, only produces small amounts of olefins, often only before reformation, raw material is carried out hydrogenation, so contain small amounts of olefins in the reformed gasoline, and the reformed gasoline olefin(e) centent of continuous reformer is higher relatively, the C that particularly wherein contains
5～C
7Cycloolefin is bigger to the benzaldehyde product quality influence.
CN1163879A has proposed a kind of method of being produced pure aromatics by reformed gasoline, earlier with the reformed gasoline selective hydrogenation, mainly make alkene, diolefine and alkatrienes selective hydrogenation in the raw material, and then the raw material after the selective hydrogenation carried out extractive distillation and/or liquid-liquid extraction, separate wherein aromatic hydrocarbons and non-aromatics.Though this method can effectively be removed the alkene in the raw material, also the benzene hydrogenation in the raw material might be become hexanaphthene, thereby reduce the benzene yield.In addition, the investment that the increase hydrogenation unit needs in abstraction distillation system is very big, and device process cost height needs to consume the hydrogen resource, so the practical application of this method is restricted.
CN1393507A has proposed a kind of method of extractive distillation aromatics separation and the double solvents of use, and double solvents comprises main solvent and solubility promoter.When this double solvents is used for cracking hydrogenated gasoline extractive distillation recovery benzene, can significantly relax the solvent recuperation operational condition, improve aromatic recovery rate, obtain high-quality purified petroleum benzin, but when raw material is CONTINUOUS REFORMER generation oil, the pickling chromatic number of benzaldehyde product is defective, even by clay-filtered, when clay tower charging mass space velocity is 0.5 hour
-1The time, in device about two weeks of running, benzaldehyde product pickling chromatic number will be defective greater than 3, needs to change carclazyte, brings the operation fluctuation, increased production cost.
Summary of the invention
The purpose of this invention is to provide a kind of from the higher hydrocarbon raw material of olefin(e) centent the method for extracting rectifying and separating benzene, this method is separated the benzaldehyde product stable in properties that obtains, and does not increase the energy consumption of extracting rectifying process substantially.
The method of extracting rectifying and separating benzene provided by the invention comprises the steps:
(1) will contain the middle part that the hydrocarbon mixture of alkene and benzene is introduced extractive distillation column, contact with the extraction solvent of introducing from extractive distillation column top and to carry out extracting rectifying, the benzene solvent that contains of discharging at the bottom of the extracting rectifying Tata enters solvent recovery tower Separation of Benzene and extraction solvent, and overhead stream is the discharge system after cooling off;
(2) feeding clay tower after the benzene cut condensation that the solvent recuperation column overhead is discharged makes with extra care, and then send into the flash distillation of benzene flash tank, after the part of the extraction solvent of discharging at the bottom of the solvent recovery tower enters the thermal source of benzene flash tank reboiler as reboiler, again with return extractive distillation column after another part extraction solvent mixes and recycle
(3) after the logistics condensation that the benzene flash drum overhead is discharged as benzaldehyde product, a jar end component is discharged system.
The present invention is for improving the benzaldehyde product quality of stability, guarantee that benzaldehyde product has qualified pickling chromatic number, the benzene cut that extracting rectifying is obtained is with after clay-filtered, carry out flash distillation again, thereby the heavy olefins that contains in the benzene cut is retained at the bottom of the flash tank, purified petroleum benzin is discharged from the flash distillation tank deck, and flash tank heats used thermal source and is provided by the extraction solvent that solvent recovery tower reclaims, just carry out the flash distillation of benzene cut with the heat in the system, whole process energy consumption does not increase, and has just increased the benzene flash tank.With this method extracting rectifying and separating benzene, can handle the higher extracting rectifying raw material of olefin(e) centent, obtain stay-in-grade benzaldehyde product.
Description of drawings
Fig. 1 is the schematic flow sheet of extracting rectifying and separating benzene of the present invention.
Embodiment
The inventive method increases the benzene flash tank in abstraction distillation system, the heavy olefins in the benzene cut after clay tower is refining is separated with benzene, thereby obtains the benzaldehyde product of stable in properties.Use the waste heat that reclaims solvent in the abstraction distillation system to provide heat in the described method, therefore increase the energy consumption that benzene flash distillation operation does not increase abstraction distillation system substantially as benzene flash tank reboiler.
For making the more effectively alkene in the Separation of Benzene cut of benzene flash tank, its pressure preferably is controlled to be 0.05～0.15MPa, preferred 75～95 ℃ of tank deck temperature, and a jar end temperature is 80～120 ℃, reflux ratio is 0～0.5.The theoretical plate number of benzene flash tank is 0～5, more preferably 2～5.
The inventive method utilizes solvent recovery tower recovered solvent heat that the required heat of benzene cut evaporation in the benzene flash tank is provided, promptly utilize the recovery solvent and the heat of the temperature head generation of the solvent that enters extractive distillation column to make the interior benzene cut evaporation of benzene flash tank, benzene wherein steams from tank deck, the heavy olefins component is then stayed at the bottom of the benzene flash tank, is regularly discharged.Describedly enter the extraction solvent of benzene flash tank reboiler and the charging mass ratio of benzene flash tank is 5～15:1, preferred 9～12:1.The extraction solvent that enters benzene flash tank reboiler accounts for 25～100% of extraction solvent total mass, and preferred 50～75%.
The theoretical plate number of extractive distillation column preferred 35～65 in the inventive method, extraction solvent is gone into preferred 80～130 ℃ of tower temperature, column bottom temperature is 140～180 ℃, tower top pressure 0.15～0.35MPa, solvent ratio (mass ratio of solvent and extracting rectifying raw material) is 3.0～6.0, and reflux ratio (mass ratio of reflux solvent and overhead product material) is 0.2～1.0.The material that cat head is discharged in the extracting rectifying operation is a non-aromatics, and non-aromatics is the discharge system after condensation, and extracting rectifying tower bottom effluent is the extraction solvent that contains benzene.
The described extraction solvent that contains benzene separates in solvent recovery tower, the benzene cut is discharged by cat head, extraction solvent is discharged at the bottom of by tower, a reboiler that enters at the bottom of the benzene flash tank provides thermal source for it, another part with enter after the solvent of benzene flash tank reboiler recirculation and return extractive distillation column and utilize again.Described solvent recovery tower is under reduced pressure operated, and suitable cat head control pressure is 0.035～0.05MPa, and tower top temperature is 50～70 ℃, and column bottom temperature is 160～185 ℃, and reflux ratio is 0.4～1.0, theoretical plate number preferred 8～28.
In the described method, the benzene cut that contains small amounts of olefins that clay tower is used for obtaining from the solvent recuperation cat head is made with extra care, with absorption alkene wherein, the alkene that contains in the extracting rectifying raw material more for a long time, to carry out flash distillation through the benzene cut after the carclazyte absorption with the inventive method, remove heavy olefins wherein, thereby increased the work-ing life of carclazyte.Described clay tower is operation under pressurization, and suitable pressure is that 0.5～1.8MPa, temperature are preferred 0.05～1.0 hour of the mass space velocity that passes through of 120～180 ℃, benzene cut
-1
The described hydrocarbon mixture of the inventive method is mainly catalytic reforming gasoline or thermo-cracking hydrogenated gasoline, wherein mainly contains benzene and C
5～C
7Alkane and a spot of alkene and naphthenic hydrocarbon.Olefin(e) centent is 1.0～8.0 quality % in the described hydrocarbon mixture, and benzene content is 15～90 quality %.
Described extraction solvent is selected from sulfone class, glycols or contains the morpholine kind compound of 7～8 carbon atoms, preferred tetramethylene sulfone, Tetraglycol 99, five glycol, N-formyl morpholine or their mixture, more preferably tetramethylene sulfone.
Describe the present invention in detail below by Fig. 1.Among Fig. 1, the hydrocarbon mixture that contains benzene and small amounts of olefins enters interchanger 101 by pipeline 1, with the extraction solvent heat exchange after pipeline 2 enters extractive distillation column 103 from the middle part.Extraction solvent enters extractive distillation column 103 by pipeline 18 from top.Through extracting rectifying, non-aromatic component is discharged from the extracting rectifying cat head, enters return tank 104 through pipeline 3, and a part passes back into extractive distillation column, and another part is by pipeline 4 discharge systems.The extraction solvent that contains benzene at the bottom of the extractive distillation column is discharged at the bottom of tower, enter solvent recovery tower 105 middle parts through pipeline 5, through underpressure distillation, the benzene cut is discharged from the solvent recuperation cat head, enter return tank 106 through pipeline 6, enter clay tower 108 by pipeline 8 through pipeline 7 after well heater 107 heating, benzene cut refining back in clay tower enters benzene flash tank 109 by pipeline 9, the benzene that tank deck obtains enters return tank 111 through pipeline 10, again by pipeline 11 discharge systems.The extraction solvent that obtains at the bottom of the solvent recovery tower is divided into two strands behind pipeline 12, one enters the thermal source of the reboiler 110 of benzene flash tank 109 as heating benzene cut by pipeline 13 by variable valve 113 controls, and then through pipeline 15 with enter pipeline 16 after another strand extraction solvent of being told by pipeline 14 mixes, enter interchanger 101 and hydrocarbon mixture heat exchange again, after pipeline 17 enters 102 temperature adjustments of aqueous solvent cooler, enter the recycle of extractive distillation column top by pipeline 18 again.The fluid level controller 112 of benzene flash tank 109 is according to the aperture of the liquid level regulating and controlling valve 113 in the jar, thereby the quantity of solvent of benzene flash tank reboiler is passed through in control, i.e. control adds heat.In actually operating, also comprise the solvent reclamation part, do not mark among Fig. 1.
Further describe the present invention below by example, but the present invention is not limited to this.
Example 1
Press the flow process of Fig. 1, with the C of reformed gasoline
6Cut is a raw material, and extracting rectifying separates purified petroleum benzin, is extraction solvent with the tetramethylene sulfone.The composition of raw material and flow see Table 1 in the extracting rectifying process, main operational condition sees Table 2, and the circular flow of solvent and heat exchange temperature see Table 3, and the extracting rectifying separating resulting sees Table 4, the benzaldehyde product pickling chromatic number that obtains after flash distillation is refining sees Table 5, and described pickling chromatic number is measured by the GB/T2012 method.
Comparative Examples
Press the method aromatics separation of example 1, different is not establish the benzene flash tank in the extracting rectifying system, the extraction solvent that obtains from solvent recovery tower directly and extractive distillation column charging heat exchange, operational condition sees Table 2, the circular flow of solvent and heat exchange temperature see Table 3, the extracting rectifying separating resulting sees Table 4, and the pickling chromatic number of the benzaldehyde product after process is clay-filtered sees Table 5.
As shown in Table 3, to reclaim the temperature that the back solvent enters extraction distillation column in order adjusting in the Comparative Examples, 135 ℃ hot solvent in the pipeline 17 to be cooled to 105 ℃ with water cooler, energy loss is huge therebetween.And made full use of the adjusted waste heat of recovery solvent after increasing benzene flash distillation operation in the example 1 of the present invention, and use it for the heat of benzene flash distillation operation to supply with, make the temperature difference before and after the aqueous solvent cooler have only 12 ℃.Table 4 whole process energy consumption shows that the benzene flash distillation operation that the inventive method increases does not increase the total energy consumption that device turns round substantially.
Table 5 data show, adopt the pickling chromatic number of the benzene that flow process of the present invention obtains qualified, and still more stable through running over a long time, thereby have increased the work-ing life of carclazyte, and having reduced the cost that frequent switching carclazyte brings increases and the operation fluctuation.And the pickling chromatic number of the benzene that the Comparative Examples that does not have a benzene flash distillation operation obtained after very short in extracting rectifying device runtime is promptly defective, needs to change carclazyte.
Example 2～3
Press Fig. 1 flow process, getting the benzene cut that the solvent recuperation cat head obtains is raw material, investigates the influence of flash distillation tank deck theoretical plate number to the extracting and separating result, and the composition of described benzene cut sees Table 6, the operational condition of clay tower and flash tank sees Table 7, separating resulting sees Table 8.
By table 8 data as can be known, when flash distillation tank deck theoretical plate number is 0 or 5, all can obtain the qualified benzaldehyde product of pickling chromatic number, but that theoretical plate number is 0 o'clock a benzene yield is on the low side.
Table 1
Table 2
Table 3
Table 4
Total heat consumption refers to extracting rectifying, benzin heating capacity sum.
Table 5
Table 6
Table 7
Table 8
Claims (8)
1. the method for an extracting rectifying and separating benzene comprises the steps:
(1) will contain the middle part that the hydrocarbon mixture of alkene and benzene is introduced extractive distillation column, contact with the extraction solvent of introducing from extractive distillation column top and to carry out extracting rectifying, the extraction solvent that contains benzene of discharging at the bottom of the extracting rectifying Tata enters solvent recovery tower Separation of Benzene and extraction solvent, and overhead stream is the discharge system after cooling off;
(2) feeding clay tower after the benzene cut condensation that the solvent recuperation column overhead is discharged makes with extra care, and then send into the flash distillation of benzene flash tank, after the part of the extraction solvent of discharging at the bottom of the solvent recovery tower enters the thermal source of benzene flash tank reboiler as reboiler, again with return extractive distillation column after another part extraction solvent mixes and recycle
(3) after the logistics condensation that the benzene flash drum overhead is discharged as benzaldehyde product, a jar end component is discharged system.
2. in accordance with the method for claim 1, it is characterized in that described benzene flash tank pressure is 0.05～0.15MPa, reflux ratio is 0～0.5, and the tank deck temperature is 75～95 ℃, and a jar end temperature is 80～120 ℃.
3. in accordance with the method for claim 2, the theoretical plate number that it is characterized in that the benzene flash tank is 0～5.
4. in accordance with the method for claim 1, it is characterized in that entering the extraction solvent of benzene flash tank reboiler and the charging mass ratio of benzene flash tank is 5～15:1.
5. in accordance with the method for claim 1, it is characterized in that the extraction solvent that enters benzene flash tank reboiler accounts for 25～75% of extraction solvent total mass.
6. in accordance with the method for claim 1, the service temperature that it is characterized in that described clay tower is that 120～180 ℃, pressure are that the mass space velocity that 0.5～1.8MPa, benzene cut pass through is 0.05～1.0 hour
-1
7. in accordance with the method for claim 1, it is characterized in that olefin(e) centent is 1.0～8.0 quality % in the described hydrocarbon mixture, benzene content is 15～90 quality %.
8. in accordance with the method for claim 1, it is characterized in that described extraction solvent is selected from tetramethylene sulfone, Tetraglycol 99, five glycol, N-formyl morpholine or their mixture.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103566620B (en) * | 2013-10-30 | 2015-06-24 | 天津市化工设计院 | Device and method for recycling light components by utilizing flash tank |
| CN111978143B (en) * | 2019-05-23 | 2023-05-05 | 中国石油化工股份有限公司 | Composite solvent for separating aromatic hydrocarbon by extractive distillation and application thereof |
| CN112209799A (en) * | 2020-10-14 | 2021-01-12 | 潍坊弘润石化科技有限公司 | Benzene-containing wastewater recycling technology |
| CN113713427A (en) * | 2021-07-28 | 2021-11-30 | 常州大学 | Method for extracting and separating aromatic hydrocarbon from alkane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994009878A1 (en) * | 1992-10-28 | 1994-05-11 | Chevron Chemical Company | High purity benzene production using extractive distillation |
| CN1260340A (en) * | 1999-06-11 | 2000-07-19 | 中国石油化工集团公司 | Method for separating arene by using extraction and rectification |
| CN1278291A (en) * | 1997-09-03 | 2000-12-27 | Hfm国际公司 | Aromatics separation process and method of retrofitting existing equipment for same |
-
2006
- 2006-02-28 CN CNB2006100080745A patent/CN100460373C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994009878A1 (en) * | 1992-10-28 | 1994-05-11 | Chevron Chemical Company | High purity benzene production using extractive distillation |
| CN1278291A (en) * | 1997-09-03 | 2000-12-27 | Hfm国际公司 | Aromatics separation process and method of retrofitting existing equipment for same |
| CN1502595A (en) * | 1997-09-03 | 2004-06-09 | Hfm���ʹ�˾ | Aromatics separation process and method of retrofitting existing equipment for same |
| CN1260340A (en) * | 1999-06-11 | 2000-07-19 | 中国石油化工集团公司 | Method for separating arene by using extraction and rectification |
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