CN1923772A - Method of extracting, rectifying and separating aromatic hydrocarbons and extracting and rectifying apparatus - Google Patents
Method of extracting, rectifying and separating aromatic hydrocarbons and extracting and rectifying apparatus Download PDFInfo
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- CN1923772A CN1923772A CN 200510093777 CN200510093777A CN1923772A CN 1923772 A CN1923772 A CN 1923772A CN 200510093777 CN200510093777 CN 200510093777 CN 200510093777 A CN200510093777 A CN 200510093777A CN 1923772 A CN1923772 A CN 1923772A
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Abstract
The invention discloses a recycling method of aromatic hydrocarbon, which comprises the following steps: inducing hydrocarbon compound from middle part of distilled tower; inducing distilled solvent from distilled tower; heating the bottom of non-aromatic hydrocarbon reflux segment; draining others out of system; distilling compound in the solvent recycling tower; separating the aromatic hydrocarbon from extracting distilled solvent; inducing separated solvent in the extracting distilled tower to recycle.
Description
Technical field
The present invention is a kind of method and a kind of extracting rectifying device that uses this method that utilizes extracting rectifying aromatics separation from hydrocarbon mixture.
Background technology
At present, utilize the technology of extracting rectifying aromatics separation from hydrocarbon mixture in industrial widespread use.This method is utilized the difference of selective solvent to each component relative volatility influence of hydro carbons, realizes that by distillation operation aromatic hydrocarbons separates with non-aromatics.Raw material adds from the extractive distillation column middle part during operation, selective solvent adds from the top of tower, non-aromatics is from removed overhead, obtain the mixture of aromatic hydrocarbons and solvent at the bottom of the tower, the solvent that contains aromatic hydrocarbons at the bottom of the tower enters solvent recovery tower again and carries out rectifying, separate obtaining aromatic hydrocarbons and solvent, solvent recycles through returning extractive distillation column after the heat exchange.Used selective solvent has glycols, tetramethylene sulfone, N-Methyl pyrrolidone (NMP) and N-formyl morpholine (NFM) etc.
Adopt different selective solvents and extracting rectifying condition, people have proposed the technology of many extracting rectifying aromatics separations.CN109143A discloses a kind of method of extracting rectifying separating hydrocarbons mixture; adopt tetramethylene sulfone or N-formyl morpholine or both mixtures as selective solvent; slective extraction distillation operation condition; make extractive distillation column in vapour-liquid-liquid three-phase operation; and, guarantee between vapour-liquid-liquid three-phase, can carry out good mass transfer by member that is provided with in the tower and filler.CN1085646C also discloses a kind of method of extracting rectifying aromatics separation, adopt tetramethylene sulfone as selective solvent, the operational condition of control extracting rectifying makes extractive distillation column operate in the critical state that dissolves each other, i.e. operation keeps a liquid phase, will reach and does not reach the state of two liquid phases.CN1393507A has proposed a kind of method of extracting rectifying aromatics separation and the double solvents of use, double solvents comprises main solvent, solubility promoter and properties-correcting agent, main solvent and properties-correcting agent are selected from tetramethylene sulfone, N-Methyl pyrrolidone or N-formyl morpholine respectively, but acid-basicity is opposite; Solubility promoter is selected from C
8～C
11Aromatic hydrocarbons.The effect of solubility promoter is to increase dissolving power, makes extractive distillation column operate in a liquid phase state and carries out.
Aforesaid method has the branch of single liquid phase and two liquid phases under the extractive distillation column operational condition.When the extractive distillation column operation is in a liquid phase state, can adopt conventional tray column structure, operating process is stable, but the tray column long-term operation.When extractive distillation column operates in two liquid phase states, then can selective solvent selectivity height, operational condition that energy consumption is low, but require on the equipment to adopt filler and special component is set, to guarantee in the tower excellent contact, mass transfer between vapour-liquid-liquid three-phase, otherwise separating effect can be very poor, and fluctuation of service, bumping can occur towards tower when serious, solvent coking and other impurity also can make the separating effect variation in the accumulation of packing layer in addition, can not guarantee long-term operation.In actual production, the key factor that device is stable, long-term operation determines its economic benefit often, thereby industrial extracting rectifying process is to operate under a liquid phase state mostly at present.No matter extractive distillation column is operated under which kind of state, and it all is the unfavorable factor that influences the extracting rectifying effect that extracting rectifying cat head non-aromatics refluxes.The effect that non-aromatics refluxes only is the trace solvent that reclaims wherein, but, non-aromatics increases along with refluxing, extracting rectifying section solvent strength descends, selective separation effect to aromatic hydrocarbons and non-aromatics also descends thereupon, the extracting rectifying section more trends towards two liquid phase states simultaneously, has strengthened the unstable of operation.
US5,310,480 have proposed the method for the extracting rectifying aromatics separation that a kind of non-aromatics do not reflux, this method only adopts the extractive distillation column of a band reboiler that the aromatic hydrocarbons in the raw material is separated with non-aromatics, the solvent droplets that the gas phase that cat head steams is at first emanated out and carried secretly through cyclonic separator, gas phase enters condensate cooler again and obtains the non-aromatics liquid-phase product, contain aromatic hydrocarbons from the middle side line extraction of extractive distillation column, the gas phase of water and trace solvent enters cyclonic separator with one recirculated water, enters condensate cooler again through the gas phase behind washing and the centrifugal segregation and obtains the aromatic hydrocarbons liquid-phase product.Used solvent is aqueous tetramethylene sulfone or glycols solvent.This method has only been carried out the one-level stream-liquid phase balance for solvent in the gas phase and non-aromatics, so solvent is higher in the non-aromatics product, and not only solvent loss strengthens, and influences the non-aromatics quality product.
Summary of the invention
The purpose of this invention is to provide and a kind ofly reclaim the method for aromatics separation by extracting rectifying from hydrocarbon mixture, this method can effectively improve the selectivity and the operational stability of extracting rectifying.
The method of utilizing extracting rectifying from hydrocarbon mixture, to reclaim aromatic hydrocarbons of the present invention, comprise hydrocarbon mixture is introduced from the middle part of extractive distillation column, extraction distillation solvent is introduced from the top of extractive distillation column, and in the bottom of this tower non-aromatics reflux section thermal source is set and heats, the control extractive distillation column is operated under the extracting rectifying condition, a cat head non-aromatics part refluxes, all the other discharge systems, the mixture that obtains aromatic hydrocarbons and solvent at the bottom of the tower enters solvent recovery tower and carries out rectifying, separate obtaining aromatic hydrocarbons and extraction distillation solvent, the solvent that will obtain after will separating is again introduced extractive distillation column and is recycled.
The inventive method is by adopting in extractive distillation column non-aromatics reflux section bottom the suitably method of heating, make that the liquid phase that enters the extracting rectifying section is extraction distillation solvent substantially, thereby the non-aromatics of effectively avoiding cat head refluxes and enters the extracting rectifying section, bring into play the effect of extracting rectifying section selective solvent aromatics separation and non-aromatics to greatest extent, improve the selectivity and the operational stability of extraction distillation solvent.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
Extractive distillation column colvent inlet to top of tower is divided into the non-aromatics reflux section of extractive distillation column in the inventive method, and the colvent inlet is following to be the extracting rectifying section.At the non-aromatics reflux section, the non-aromatics by trim the top of column makes a small amount of solvent that wherein contains separate with non-aromatics, non-aromatics evaporation and discharge from cat head in this section because boiling point is low, and extraction distillation solvent then flows into the extracting rectifying section under the colvent inlet.The inventive method is provided with thermal source in extractive distillation column non-aromatics reflux section bottom, suitably improve the temperature of reflux section bottom, make the trim the top of column non-aromatics exist only in the non-aromatics reflux section, substantially avoided the backflow non-aromatics to flow into the extracting rectifying section, improved extracting rectifying section solvent strength, thereby strengthened the effect of extracting rectifying section selective separation aromatic hydrocarbons and non-aromatics, and can make the operation of extracting rectifying section more stable.
Extraction distillation solvent described in the inventive method is selected from tetramethylene sulfone, glycol ether, triglycol, Tetraglycol 99, N-formyl morpholine or N-Methyl pyrrolidone; it also can be the double solvents that comprises main solvent and solubility promoter; wherein main solvent is selected from tetramethylene sulfone, glycol ether, triglycol, Tetraglycol 99, N-formyl morpholine or N-Methyl pyrrolidone, and solubility promoter is selected from C
8～C
11In the aromatic hydrocarbons any one or two kinds, a kind of aromatic hydrocarbons herein refers to have the aromatic hydrocarbons of same carbon number, as C
8The both single C of aromatic hydrocarbons
8Aromatic hydrocarbons as ethylbenzene, o-Xylol, also can be blended C
8Aromatic hydrocarbons, as contain the xylol of different isomerization body.The content of solubility promoter is 5～30 quality % in the described double solvents.
The working pressure of described extractive distillation column is 0.1～0.35MPa, it is 60～130 ℃ that solvent is gone into the tower temperature, non-aromatics reflux section bottom temp is 100～160 ℃, preferred 120～150 ℃, column bottom temperature is 140～180 ℃, theoretical plate number is 20～50, and solvent is 2.0～7.0 with the ratio (being solvent ratio) of raw materials quality flow.The trim the top of column ratio is 0.1～3.0.The tower top pressure of solvent recovery tower is 0.03～0.08MPa, and column bottom temperature is 170～180 ℃, and theoretical plate number is 10～20, and the trim the top of column ratio is 0.5～3.0.
Solvent is preferably greater than 80 quality % greater than 60 quality % in the effusive liquid in described non-aromatics reflux section bottom.
The described thermal source that is used to heat extractive distillation column non-aromatics reflux section can be from the engineering thermal source of abstraction distillation system outside or utilizes the waste heat of abstraction distillation system circulating solvent, preferably uses reboiler to heat.
The device that utilizes extracting rectifying from hydrocarbon mixture, to reclaim aromatic hydrocarbons of the present invention, comprise the extractive distillation column and the solvent recovery tower of polyphone each other, the middle part of described extractive distillation column is provided with the colvent inlet pipe, non-aromatics reflux section bottom, extractive distillation column internal solvent inlet tube top is provided with reboiler, the top of extractive distillation column is provided with non-aromatics outlet pipe and return line, the bottom is provided with reboiler and aromatic hydrocarbons outlet pipe, and the aromatic hydrocarbons outlet pipe links to each other with the middle part of solvent recovery tower.
In the described device, the non-aromatics reflux section in the extractive distillation column is provided with 1～10 grade of vapour-liquid contact column plate, and the non-aromatics at this section place is fully separated with a small amount of solvent, to guarantee not contain solvent in the cat head non-aromatics.
Hydrocarbon mixture of the present invention is the hydro carbons that contains 5～10 carbon atoms, and wherein aromaticity content is preferably greater than 30 quality % greater than 15 quality %.
Below in conjunction with Fig. 1 the inventive method is described.The hydrocarbon mixture that contains aromatic hydrocarbons enters interchanger 3 by pipeline 1, enters extractive distillation column 4 middle parts after the heat exchange, and extraction distillation solvent enters extractive distillation column 4 through pipeline 2 from top.Extractive distillation column is the non-aromatics reflux section more than the colvent inlet, and this section is provided with 1～10 grade of vapour-liquid contact column plate, and its bottom is provided with reboiler 5, and the backflow non-aromatics is used to vaporize.The reboiler that is provided with at the bottom of the extractive distillation column provides heat, in tower, form the vapour-liquid counter current contact, non-aromatics in the hydrocarbon mixture is discharged by overhead line 6, enter lime set jar 8 after entering condenser 7 condensations, cooling, wherein a part passes back into extractive distillation column 4 through pipeline 9, and rest part is sent system as the non-aromatics product through pipeline 10.The solvent of arene rich enters solvent recovery tower 13 middle parts through pipeline 12 at the bottom of the tower, establishes reboiler 20 at the bottom of the tower, carries out fractionation by distillation aromatic hydrocarbons and solvent under reduced pressure, and lime set jar 17 apical grafting vacuum systems 16 are kept solvent recovery tower and under reduced pressure operated.The aromatic hydrocarbons that contains in the solvent is discharged through pipeline 14 by cat head, enter condenser 15 and enter lime set jar 17 through condensation, cooling, wherein a part passes back into solvent recovery tower 13 through pipeline 18, all the other are through pipeline 19 discharge systems, solvent is discharged by tower bottom tube line 21, loops back extractive distillation column 4 by pipeline 2 after heat exchange.
Further specify the present invention below by example, but the present invention is not limited to this.
Example 1
With C
6Cut is the extracting rectifying raw material, and its composition sees Table 1, presses flow process separation benzene and the non-aromatics wherein of Fig. 1, and used extraction distillation solvent is tetramethylene sulfone and o-Xylol, and each tower operational condition sees Table 2, reclaims product quality indicator and sees Table 3.
Comparative Examples 1
Press the method separation of C of CN1393507A
6Benzene in the cut and non-aromatics, the method Separation of Benzene and the non-aromatics of promptly pressing example 1, but reboiler is not established in extractive distillation column non-aromatics reflux section bottom, and each tower operational condition sees Table 2, reclaims product quality indicator and sees Table 3.
Can find out by table 2 example 1 and the data of Comparative Examples 1, after extractive distillation column non-aromatics reflux section adopts intermediate reboiler, non-aromatics reflux section bottom temp is brought up to 135 ℃ by 102 ℃ of Comparative Examples 1, the liquid phase that makes the non-aromatics reflux section flow into the extracting rectifying section is mainly solvent, substantially avoid non-aromatics to reflux and entered the extracting rectifying section, the selectivity and the operational stability of extracting rectifying section have been improved, allow cat head to adopt more non-aromatics to reflux simultaneously and improve solvent recovery effect, promptly reflux ratio increases.Table 3 data presentation is compared with Comparative Examples 1, and example 1 gained aromatic hydrocarbon product purity is higher, and yield is higher, and the solvent in the non-aromatics product reduces greatly, has reduced solvent loss.
Example 2
With C
6～C
8Cut is the extracting rectifying raw material, and its composition sees Table 1, by the flow process of Fig. 1 benzene is wherein separated with non-aromatics with toluene, and used extraction distillation solvent is a tetramethylene sulfone, and adds the water of 1 quality %.Each tower operational condition sees Table 2, reclaims product quality indicator and sees Table 3.
Comparative Examples 2
Get the raw material of example 2, press US5,310,480 method is separated BTX aromatics (benzene, toluene) and non-aromatics wherein, and used extraction distillation solvent and each tower operational condition see Table 2, reclaims product quality indicator and sees Table 3.
By table 2, table 3 data as can be known, example 2 adopts non-aromaticss to reflux to reclaim the solvent in the non-aromatics gas phase, and by the intermediate reboiler heating, the disadvantageous effect of having avoided non-aromatics to reflux the extracting rectifying section is caused substantially.Comparative Examples 2 non-aromaticss do not reflux, cat head non-aromatics steam is at first removed the solvent droplets of carrying secretly through cyclonic separator, and then carry out condensation cooling and obtain the non-aromatics product, because only carried out a thermodynamics and balanced each other, solvent not only loses solvent up to 170 μ g/kg in the non-aromatics product, and increased the sulphur content of product, have a strong impact on non-aromatic quality product, and solvent is extremely low in the non-aromatic product of example 2, does not lose solvent substantially.
Table 1
| Form quality % | C 6Cut | C 6～C 8Cut |
| Non-aromatics C 5 - C 6 C 7 C 8 +Aromatic hydrocarbons, C 6 C 7 C 8 C 9 | 4.0 38.7 17.0 0.0 40.3 0.0 0.0 0.0 | 2.2 36.6 12.2 4.1 23.9 17.6 3.4 0.0 |
| Amount to | 100.00 | 100.00 |
Table 2
| Project | Example 1 | Comparative Examples 1 | Example 2 | Comparative Examples 2 |
| Solvent composition, quality % tetramethylene sulfone o-Xylol water extractive distillation column theoretical plate number tower top pressure, the MPa solvent is gone into the tower temperature, temperature at the bottom of ℃ non-aromatics reflux section, ℃ column bottom temperature, ℃ solvent ratio reflux ratio solvent recovery tower theoretical plate number tower top pressure, the MPa column bottom temperature, ℃ reflux ratio (R/D) water stripping/solvent, ton/ton | 87 13 0 32 0.16 100 135 165 4.0 0.8 12 0.06 175 2 - | 87 13 0 32 0.16 100 102 165 4.0 0.5 12 0.06 175 2 - | 99 0 1 40 0.15 80 130 145 2.5 0.15 12 0.05 175 0.5 0.020 | 97.7 0 2.3 40 0.15 56 - - 1.85 0 - - - - 0.063 |
Table 3
| Project | Example 1 | Comparative Examples 1 | Example 2 | Comparative Examples 2 |
| Product yield, foreign matter content non-aromatics in the quality % aromatic hydrocarbons aromatic hydrocarbon product, μ g/kg solvent, foreign matter content aromatic hydrocarbons in the μ g/kg non-aromatics product, the g/100g solvent, μ g/kg | 99.9 100 ＜2 0.05 5 | 99.7 800 ＜2 0.2 50 | 99.9 500 ＜2 0.1 ＜2 | 100 500 - 0.0 170 |
Claims (11)
1, a kind of method of utilizing extracting rectifying from hydrocarbon mixture, to reclaim aromatic hydrocarbons, comprise hydrocarbon mixture is introduced from the middle part of extractive distillation column, extraction distillation solvent is introduced from the top of extractive distillation column, and in the bottom of this tower non-aromatics reflux section thermal source is set and heats, the control extractive distillation column is operated under the extracting rectifying condition, a cat head non-aromatics part refluxes, all the other discharge systems, the mixture that obtains aromatic hydrocarbons and solvent at the bottom of the tower enters solvent recovery tower and carries out rectifying, separate obtaining aromatic hydrocarbons and extraction distillation solvent, the solvent that will obtain after will separating is again introduced extractive distillation column and is recycled.
2, in accordance with the method for claim 1, it is characterized in that described extraction distillation solvent is selected from tetramethylene sulfone, glycol ether, triglycol, Tetraglycol 99, N-formyl morpholine or N-Methyl pyrrolidone.
3, in accordance with the method for claim 1; it is characterized in that described extraction distillation solvent is the double solvents that comprises main solvent and solubility promoter; wherein main solvent is selected from tetramethylene sulfone, glycol ether, triglycol, Tetraglycol 99, N-formyl morpholine or N-Methyl pyrrolidone, and solubility promoter is selected from C
8～C
11In the aromatic hydrocarbons any one or two kinds.
4, in accordance with the method for claim 3, the content that it is characterized in that solubility promoter in the double solvents is 5～30 quality %.
5, in accordance with the method for claim 1, the pressure that it is characterized in that described extractive distillation column is 0.1～0.35MPa, it is 60～130 ℃ that solvent is gone into the tower temperature, non-aromatics reflux section bottom temp is 100～160 ℃, column bottom temperature is 140～180 ℃, theoretical plate number is 20～50, and solvent is 2.0～7.0 with the ratio of raw materials quality flow, and the trim the top of column ratio is 0.1～3.0; The tower top pressure of solvent recovery tower is 0.03～0.08MPa, and column bottom temperature is 170～180 ℃, and theoretical plate number is 10～20, and the trim the top of column ratio is 0.5～3.0.
6, in accordance with the method for claim 5, the temperature that it is characterized in that described non-aromatics reflux section bottom is 120～150 ℃.
7, in accordance with the method for claim 1, it is characterized in that solvent is greater than 60 quality % in the effusive liquid in non-aromatics reflux section bottom.
8, in accordance with the method for claim 1, it is characterized in that described thermal source be selected from reboiler, from the engineering thermal source of abstraction distillation system outside or utilize the waste heat of abstraction distillation system circulating solvent.
9, in accordance with the method for claim 1, it is characterized in that described hydrocarbon mixture is the hydro carbons that contains 5～10 carbon atoms, wherein aromaticity content is greater than 15 quality %.
10, a kind of device that utilizes extracting rectifying from hydrocarbon mixture, to reclaim aromatic hydrocarbons, comprise the extractive distillation column and the solvent recovery tower of polyphone each other, the middle part of described extractive distillation column is provided with the colvent inlet pipe, non-aromatics reflux section bottom, extractive distillation column internal solvent inlet tube top is provided with reboiler, the top of extractive distillation column is provided with non-aromatics outlet pipe and return line, the bottom is provided with reboiler and aromatic hydrocarbons outlet pipe, and the aromatic hydrocarbons outlet pipe links to each other with the middle part of solvent recovery tower.
11, in accordance with the method for claim 10, it is characterized in that the non-aromatics reflux section is provided with 1～10 grade of vapour-liquid contact column plate in the described extractive distillation column.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101875592A (en) * | 2009-04-30 | 2010-11-03 | 中国石油化工股份有限公司 | Regeneration method of extracting solvent for extracting, rectifying and separating styrene |
| CN102405084A (en) * | 2009-04-21 | 2012-04-04 | 朗盛德国有限责任公司 | Method for separating aromatic compounds |
| CN103864554A (en) * | 2014-04-09 | 2014-06-18 | 天津市昊永化工科技有限公司 | Method for extracting, rectifying and separating alkane, olefin and arene from hydrocarbon mixture |
| CN105732292A (en) * | 2016-03-31 | 2016-07-06 | 中山大学 | Sulfolane aromatic hydrocarbon extraction distillation device with half-lean solution cycle logistics |
| CN107778127A (en) * | 2017-08-30 | 2018-03-09 | 中国石油化工股份有限公司 | A kind of double solvents for Sulfolane Extraction separated benzene and use method |
| CN111348981A (en) * | 2019-12-24 | 2020-06-30 | 国家能源集团煤焦化有限责任公司 | Crude benzene hydrofining method and device |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2648638A1 (en) * | 1976-10-27 | 1978-05-03 | Metallgesellschaft Ag | METHOD FOR INCREASING THE YIELD OF AROMATES IN EXTRACTIVE DISTILLATION |
| CN1083819C (en) * | 1999-06-11 | 2002-05-01 | 中国石油化工集团公司 | Method for separating arene by using extraction and rectification |
| GB2396610B (en) * | 2002-12-23 | 2006-09-20 | China Petroleum & Chemical | A process for separating aromatics by extractive distillation and a composite solvent used therein |
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| CN102405084A (en) * | 2009-04-21 | 2012-04-04 | 朗盛德国有限责任公司 | Method for separating aromatic compounds |
| CN102405084B (en) * | 2009-04-21 | 2015-09-30 | 朗盛德国有限责任公司 | For separating of the method for aromatic compound |
| CN101875592A (en) * | 2009-04-30 | 2010-11-03 | 中国石油化工股份有限公司 | Regeneration method of extracting solvent for extracting, rectifying and separating styrene |
| CN101875592B (en) * | 2009-04-30 | 2013-07-31 | 中国石油化工股份有限公司 | Regeneration method of extracting solvent for extracting, rectifying and separating styrene |
| CN103864554A (en) * | 2014-04-09 | 2014-06-18 | 天津市昊永化工科技有限公司 | Method for extracting, rectifying and separating alkane, olefin and arene from hydrocarbon mixture |
| CN103864554B (en) * | 2014-04-09 | 2015-09-30 | 天津市昊永化工科技有限公司 | The method of separation of extractive distillation alkane, alkene and aromatic hydrocarbons from hydrocarbon mixture |
| CN105732292A (en) * | 2016-03-31 | 2016-07-06 | 中山大学 | Sulfolane aromatic hydrocarbon extraction distillation device with half-lean solution cycle logistics |
| CN105732292B (en) * | 2016-03-31 | 2018-04-06 | 中山大学 | A kind of sulfolane aromatic hydrocarbons extraction distilling apparatus with semi lean solution circulation logistics |
| CN107778127A (en) * | 2017-08-30 | 2018-03-09 | 中国石油化工股份有限公司 | A kind of double solvents for Sulfolane Extraction separated benzene and use method |
| CN111348981A (en) * | 2019-12-24 | 2020-06-30 | 国家能源集团煤焦化有限责任公司 | Crude benzene hydrofining method and device |
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