CN204689922U - The device of thiophene is extracted before coking crude benzene hydrogenation - Google Patents
The device of thiophene is extracted before coking crude benzene hydrogenation Download PDFInfo
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Abstract
Extract the device of thiophene before the utility model discloses coking crude benzene hydrogenation, device comprises crude benzol cut cutter unit, extracting rectifying unit, thiophene refined unit.Adopt partitioned column by de-for benzene gently together with de-heavy two pre-separation PROCESS COUPLING, then reclaim the thiophene in benzene by extraction fractional distillation, crude benzol cut cutter unit adopts partitioned column technology, the thick purified petroleum benzin of side take-off on the right side of dividing plate; Extracting rectifying unit adopts side line tower technology, the thick thiophene of side line overhead extraction; Thiophene refined unit is batch fractionating tower; Optimize existing benzene hydrogenation process flow process, reduce hydrogen consumption, obtain purity more than 99.6% thiophene, and thiophene content in benzene is reduced to less than 0.1%, can be the hydrogen usage of follow-up benzene hydrogenation process saving about 50%.The utility model technical process is simple, facility investment is little, energy consumption is low, greatly reduces the generation of hydrogenation byproduct hydrogen sulfide, significantly improves economic benefit and the environmental benefit of crude benzole hydrogenation manufacturing enterprise.
Description
Technical field
The utility model extracts the device of thiophene before relating to a kind of coking crude benzene hydrogenation, belong to the technical field extracting thiophene from coking crude benzene.
Background technology
The main purpose of coked crude benzene refining removes the sulphur compounds such as thiophene.The component of crude benzol is very complicated, except benzene and thiophene, also containing other compositions of kind more than 100 such as toluene, dimethylbenzene, cyclopentadiene, dithiocarbonic anhydride, vinylbenzene, hexanaphthene, methylcyclohexane, naphthalenes.Wherein especially with the most difficult separation of thiophene, because itself and benzene boiling point are very close, be difficult to be separated by common method.Along with organic synthesis industry improving constantly benzene homologues specification of quality, also more and more stricter to the requirement of thiophene content in benzene.In the process for purification of current coking crude benzene, traditional acid wash due to environmental pollution serious, acid tar the reason such as cannot to be dealt carefully with and be eliminated; Crude benzole hydrogenation technique is the crude benzene refining method of current main flow, and hydrogenation method refers under certain temperature, pressure and catalysts conditions, answers, the unsaturated compound in crude benzol is converted into saturated compound by carrying out sending out with hydrogen; Carrying out desulfurization, denitrogenation, deoxygenation, is H2S, NH3, H2O etc. S, N, O cycling of elements in raw material organism.Thiophene is converted into hydro carbons and hydrogen sulfide by this technique, not only wastes this important resource of thiophene, but also adds environmental pollution.The new extraction fractional distillation crude benzol refining techniques risen in recent years, compared with hydrogenation method, investment more economizes, and technique is safer, and can also the thiophene of unit take-back cost costliness, but when hydrogenation production capacity surplus, marketing situation is unsatisfactory.If extraction fractional distillation can be combined with hydrodesulfurization, before crude benzole hydrogenation is refining, first reclaims thiophene, then not only can obtains higher economic benefit, also by obtaining higher environmental benefit, believing and promotion crude benzole hydrogenation industry is carried out a technology upgrading.
Thiophene is colourless low-viscosity (mobile) liquid, and micro-have benzene taste, is stable five member ring heterocyclic compound, has the character of aromatics, and chemical property and benzene are very close, but have higher reactive behavior.Thiophene is a kind of important industrial chemicals, is prevalent in crude benzol.Be mainly used in medicine synthesis, be also used as to produce dyestuff, synthetic resins, vulcanization accelerator, oxidation inhibitor and growth stimulant etc., there is important industrial value.
The utility model provides a kind of method of system, take crude benzol as raw material, first with partitioned column to carrying out cut cutting, obtain the mixture of benzene and thiophene, again through extractive distillation column extraction benzene, thiophene content in benzene is down to less than 0.1%, the thick thiophene of side take-off, eventually passes after refining and obtain highly purified thiophene.
Compared with traditional benzene refining process, the utility model adopts partitioned column to replace two benzene towers (weight-removing column) and primary tower (lightness-removing column), utilize partitioned column to be thermodynamically equivalent to the effect of complete thermal coupled rectifying tower, realize the object reducing facility investment and reduce energy expenditure.
The extracting rectifying genealogy of law utilizes polarity difference faint between benzene and thiophene, by adding the extraction agent that can be recycled in rectifying, increases relative volatility between the two, solves the problem that benzene is separated with thiophene difficulty.After reclaiming thiophene by this method, can be the hydrogen usage of follow-up benzene hydrogenation process saving about 50%, and reduce hydrogen internal circulating load and hydroprocessing expense.It is few that the method has facility investment, and operational condition is gentle, the advantage such as high financial profit and non-environmental-pollution.
Summary of the invention
The purpose of this utility model extracts the device of thiophene before there are provided a kind of coking crude benzene hydrogenation, this facility investment is few, operational condition is gentle, the advantage such as high financial profit and non-environmental-pollution.The method utilizes partitioned column taken off gently by benzene and together with de-heavy two pre-separation PROCESS COUPLING, then removed the thiophene in benzene by extracting rectifying, optimize existing benzene hydrogenation process flow process, reduce hydrogen consumption.
For achieving the above object, the utility model adopts following technical scheme to realize:
Extract a device for thiophene before coking crude benzene hydrogenation, comprise rough segmentation tower, extractive distillation column, side line tower and thiophene treating tower; It is characterized in that rough segmentation tower is partitioned column, and be provided with crude benzol logistics opening for feed and backflow material inlet, the benzene of partitioned column side take-off and thiophene cut enter extractive distillation column opening for feed, and tower top is provided with condenser; Extracting rectifying column overhead is provided with refluxing opening, top is provided with extraction agent import, bottom is provided with side line tower gas phase extraction mouth and side line tower liquid-phase reflux mouth, tower top is provided with condenser, reboiler is provided with at the bottom of tower, discharge port at the bottom of tower is connected to tower top extractant feed mouth, and gas phase extraction mouth is connected to side line tower opening for feed; Side line top of tower is provided with refluxing opening, and bottom is provided with gas-phase feed mouth and liquid-phase reflux mouth, and tower top is provided with condenser, and overhead extraction mouth is connected to thick thiophene storage tank; Thick thiophene storage tank is provided with material inlet and outlet, and outlet is connected to thiophene treating tower tower reactor; Be connected with tower reactor bottom thiophene treating tower, top of tower is provided with condenser.
Multi-heat exchanger is provided with between rough segmentation tower and extractive distillation column, extraction mouth at the bottom of extractive distillation column tower is connected to the import of rough segmentation tower reboiler shell side, be connected to the import of preheater shell side successively, be connected to the import of extractive distillation column feed preheater shell side, finally by being connected to extractive distillation column extractant feed mouth after water cooler.
The utility model creates the advantage that has and positively effect is:
The utility model adopts partitioned column by de-for benzene gently together with de-heavy two pre-separation PROCESS COUPLING, and then reclaim the thiophene in benzene by extraction fractional distillation, crude benzol cut cutter unit adopts partitioned column technology, the thick purified petroleum benzin of side take-off on the right side of dividing plate; Extracting rectifying unit adopts side line tower technology, the thick thiophene of side line overhead extraction; Thiophene refined unit is batch fractionating tower; Optimize existing benzene hydrogenation process flow process, reduce hydrogen consumption, obtain purity more than 99.6% thiophene, and thiophene content in benzene is reduced to less than 0.1%, can be the hydrogen usage of follow-up benzene hydrogenation process saving about 50%.The utility model technical process is simple, facility investment is little, energy consumption is low, by increasing several tower before crude benzole hydrogenation, very worthy thiophene can be extracted, and hydrogenation technique load can be reduced, reduce hydrogen consumption, greatly reduce the generation of hydrogenation byproduct hydrogen sulfide, significantly improve economic benefit and the environmental benefit of crude benzole hydrogenation manufacturing enterprise.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the utility model adopts
C1-rough segmentation tower, C2-extractive distillation column, C3-thiophene treating tower, C4-side line tower, E1-C1 tower condenser, E2-C1 tower reboiler, E3-C1 tower preheater, E4-C2 tower condenser, E5-C2 tower reboiler, E6-C2 tower preheater, E7-extraction agent water cooler, E8-C4 tower condenser, E9-C3 tower condenser, E10-C3 thiophene treating tower tower reactor, the thick thiophene storage tank of V1-, the import of F-extraction agent, 1-crude benzol, 2-starting fraction, 3-toluene, dimethylbenzene etc. remove hydrogenation, the thick thiophene of 4-, 5-thiophene product, 6-transition component, 7-takes off thiophene benzene and removes hydrogenation.
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in further detail:
As shown in Figure 1: the device extracting thiophene before a kind of coking crude benzene hydrogenation, comprises rough segmentation tower, extractive distillation column, side line tower, thiophene treating tower, reclaim the object of thiophene before realizing coking crude benzene hydrogenation.It is characterized in that rough segmentation tower C1 is partitioned column, and be provided with crude benzol logistics 1 opening for feed and backflow material inlet, the benzene of partitioned column side take-off and thiophene cut enter extractive distillation column C2 opening for feed, and tower top is provided with condenser; Extractive distillation column C2 tower top is provided with refluxing opening, top is provided with extraction agent import, bottom is provided with side line tower gas phase extraction mouth and side line tower liquid-phase reflux mouth, tower top is provided with condenser, reboiler is provided with at the bottom of tower, tower bottom outlet is connected to tower top extractant feed mouth, and gas phase extraction mouth is connected to side line tower C4 opening for feed; Side line tower C4 top is provided with refluxing opening, and bottom is provided with gas-phase feed mouth and liquid-phase reflux (entering extractive distillation column) mouth, and tower top is provided with condenser, and overhead extraction mouth is connected to thick thiophene storage tank V1; Thick thiophene storage tank V1 is provided with material inlet and outlet, and outlet is connected to thiophene treating tower tower reactor E10; Be connected with tower reactor E10 bottom thiophene treating tower C3, top of tower is provided with condenser.
In order to realize effective utilization of heat, multi-heat exchanger is provided with between rough segmentation tower C1 and extractive distillation column C2, multi-heat exchanger is provided with between rough segmentation tower C1 and extractive distillation column C2, extraction mouth at the bottom of extractive distillation column C2 tower is connected to the import of rough segmentation tower C1 reboiler E2 shell side, then the import of preheater E3 shell side is connected to, be connected to the import of extractive distillation column C2 feed preheater E6 shell side, finally by being connected to extractive distillation column C2 extractant feed mouth after water cooler E7.Bottom extractive distillation column C2, extraction extraction agent is first as the thermal source of C1 tower reboiler E2, then through preheater E3 preheating crude benzol logistics 1, then preheating C2 tower charging in C2 tower feed preheater E6, enters C2 tower extractant feed mouth after cooling finally by condenser E7.
First crude benzol enters rough segmentation tower C1, overhead extraction starting fraction, the components such as extraction toluene, dimethylbenzene at the bottom of tower, and at the bottom of tower top and tower, production sends to hydrogenation respectively, and the thick purified petroleum benzin of side take-off sends into extractive distillation column C2 middle and lower part; The extraction of C2 top takes off thiophene benzene and sends to hydrogenation, bottom extraction extraction agent, returns to extractive distillation column C2 top and recycle after multi-stage heat exchanger, extractive distillation column C2 middle and lower part gas phase production approaching side transmission tower C4; The thick thiophene of C4 overhead extraction, liquid-phase reflux at the bottom of tower is to C2 tower; Thick thiophene enters in thiophene treating tower C3 and purifies, and obtains product thiophene 5 and transition component 6.
Rough segmentation tower adopts partitioned column, and crude benzol enters rough segmentation tower dividing plate left side central portion after preheater preheats.This tower normal pressure operate continuously, the component that overhead extraction is lighter than benzene, main component is dithiocarbonic anhydride, cyclopentadiene, pentamethylene and methylcyclopentane.Extraction toluene, dimethylbenzene, vinylbenzene, ethylbenzene, naphthalene at the bottom of tower and to wash in benzene process residual washing oil.On the right side of dividing plate, side take-off benzene and thiophene send into extractive distillation column bottom as raw material.
By the benzene of rough segmentation tower side take-off and thiophene after preheater preheats, enter extractive distillation column middle and lower part.This tower negative pressure operate continuously, cycling extraction agent enters this tower top, and extraction agent used is: one or several the mixture in ethylene glycol, glycol ether, triglycol, N-Methyl pyrrolidone, N-N-formyl morpholine N-, gamma-butyrolactone, tetramethylene sulfone.Extractant feed amount is 6 ~ 20 times (mass ratioes) of material quantity.The purified petroleum benzin cut that overhead extraction thiophene content is less than 0.1%.Obtain the extraction agent that thiophene content is not more than 5mg/kg at the bottom of tower, through with rough segmentation tower reboiler, rough segmentation tower preheater, the heat exchange of extractive distillation column preheater after, be cooled with circulating water less than 80 DEG C, enter extractive distillation column top and recycle.
The mixed fraction of thiophene, benzene, toluene and extraction agent is contained, bottom approaching side transmission tower 4 by the extraction of extractive distillation column side line gas phase.The operate continuously of side line tower negative pressure, only establishes condenser, does not establish reboiler, and overhead vapours is after condensation, and partial reflux, part extraction enters thick thiophene storage tank as thick thiophene (composition is thiophene and toluene mainly, containing a small amount of benzene).
Thiophene treating tower atmosphere intermission operates, and the thick thiophene from thick thiophene storage tank enters tower reactor, and through batch fractionating, after a small amount of front-end volatiles benzene of extraction and transition component, during tower top temperature about 84 DEG C, extraction content is not less than the thiophene product of 99.6%.
Embodiment 1
1. crude benzol cut cutter unit: crude benzol (containing benzene 74.5%, thiophene 1%, toluene 12.8%, dithiocarbonic anhydride 2.03%, cyclopentadiene 0.83%, p-Xylol 0.63%, m-xylene 1.66%, o-Xylol 0.53%, vinylbenzene 1.12%, indenes 1.11%, naphthalene 3.79%) through preheater preheats to 94.6 DEG C, after partial gasification, enter on the left of rough segmentation tower dividing plate.This tower atmospheric operation, overhead extraction light constituent (containing benzene 30.7%, thiophene 0.2%, dithiocarbonic anhydride 49.1%, cyclopentadiene 20%), tower top temperature 51.7 DEG C; The thick purified petroleum benzin of extraction (containing benzene 96.7%, thiophene 1.3%, toluene 1.9%) on the right side of dividing plate, temperature 81.7 DEG C; Extraction toluene, dimethylbenzene and heavy benzene (containing benzene 2mg/kg, toluene 56.2%, p-Xylol 3.1%, m-xylene 8.2%, o-Xylol 2.6%, vinylbenzene 5.6%, indenes 5.5%, naphthalene 18.8%) at the bottom of tower, column bottom temperature 126.1 DEG C.At the bottom of tower top and tower, hydrogenation workshop section is sent in extraction.
2. extracting rectifying unit: from the thick purified petroleum benzin of rough segmentation tower side line through preheater preheats to 61.4 DEG C, be gasified totally (because of extractive distillation column decompression operation), enters extractive distillation column middle and lower part.The cycling extraction agent NMP of 6 times of inlet amounies is cooled to 70 DEG C to enter this tower top through water cooler.This tower top pressure-0.05MPa (G), tower top temperature 59.6 DEG C, overhead extraction benzene cut logistics (containing benzene 99.9%, thiophene 831mg/kg) goes hydrogenation as raw material.Extraction agent after extraction regeneration at the bottom of tower, through rough segmentation tower reboiler, rough segmentation tower preheater, the heat exchange of extractive distillation column preheater, then after extraction agent water cooler is cooled with circulating water 70 DEG C, return to extractive distillation column top.
From the extractive distillation column bottom thick thiophene cut of side line gas phase extraction to side line tower.Side line decompressing and continuous operates, and tower top pressure-0.045MPa (G), temperature 81.3 DEG C, overhead vapours (benzene 0.5%, thiophene 42.9%, toluene 56.6%) passes back into side line top of tower through condensation rear section, and thick thiophene storage tank is entered in part extraction.Liquid phase extraction backflow at the bottom of side line tower tower enters extractive distillation column bottom.
3. thiophene refined unit: the thick thiophene from storage tank heats through thiophene treating tower tower reactor, enters thiophene treating tower.Through batch fractionating, after a small amount of front-end volatiles benzene of extraction and transition component, the thiophene product of extraction content 99.6% during tower top temperature about 84 DEG C.
Embodiment 2
1. crude benzol cut cutter unit: crude benzol (containing benzene 74.2%, thiophene 1.3%, toluene 12.5%, dithiocarbonic anhydride 2%, cyclopentadiene 1%, p-Xylol 0.7%, m-xylene 1.65%, o-Xylol 0.65%, vinylbenzene 1.1%, indenes 1.1%, naphthalene 3.8%) through preheater preheats to 94.6 DEG C, after partial gasification, on the left of the dividing plate entering rough segmentation tower.Rough segmentation tower atmospheric operation, tower top temperature 50.6 DEG C, overhead extraction light constituent (containing benzene 27.3%, thiophene 0.2%, dithiocarbonic anhydride 48.3%, cyclopentadiene 24.2%); The thick purified petroleum benzin of extraction (containing benzene 96.5%, thiophene 1.7%, toluene 1.8%) on the right side of dividing plate, temperature 81.7 DEG C; Extraction toluene, dimethylbenzene and heavy benzene (containing benzene 2mg/kg, toluene 55.4%, p-Xylol 3.5%, m-xylene 8.2%, o-Xylol 3.2%, vinylbenzene 5.5%, indenes 5.5%, naphthalene 18.8%) at the bottom of tower, column bottom temperature 126.4 DEG C.
2. extracting rectifying unit: thick purified petroleum benzin is through preheater preheats to 64.6 DEG C, and be gasified totally (because of extractive distillation column decompression operation), enters extractive distillation column middle and lower part.The cycling extraction agent NFM of 20 times of inlet amounies is cooled to 70 DEG C to enter this tower top through water cooler.This tower decompression operation, tower top pressure-0.06Mpa (G), tower top temperature 53.6 DEG C, overhead extraction benzene cut logistics (containing benzene 99.9%, thiophene 37mg/kg) goes hydrogenation as raw material.Extraction agent after extraction regeneration at the bottom of tower, through rough segmentation tower reboiler, rough segmentation tower preheater, the heat exchange of extractive distillation column preheater, then after extraction agent water cooler is cooled with circulating water 70 DEG C, return to extractive distillation column top.
From the extractive distillation column bottom thick thiophene cut of side line gas phase extraction to side line tower.Side line decompressing and continuous operates, tower top pressure-0.055MPa (G), temperature 74.3 DEG C, overhead vapours (benzene 277mg/kg, thiophene 48.6%, toluene 51.3%) pass back into side line top of tower through condensation rear section, thick thiophene storage tank is entered in part extraction.Liquid phase extraction backflow at the bottom of side line tower tower enters extractive distillation column bottom.
3. thiophene refined unit: the thick thiophene from storage tank heats through thiophene treating tower tower reactor, enters thiophene treating tower.Through batch fractionating, after a small amount of front-end volatiles benzene of extraction and transition component, the thiophene product of extraction content 99.7% during tower top temperature about 84 DEG C.
The device that the utility model discloses and proposes, those skilled in the art are by using for reference present disclosure, appropriate change realizes, although the utility model technology of preparing is described by preferred embodiment, person skilled obviously can change Method and Technology route as herein described or reconfigure not departing from the utility model content, spirit and scope, realizes final technology of preparing.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in the utility model spirit, scope and content.
Claims (2)
1. extract a device for thiophene before coking crude benzene hydrogenation, comprise rough segmentation tower, extractive distillation column, side line tower and thiophene treating tower; It is characterized in that rough segmentation tower is partitioned column, and be provided with crude benzol logistics opening for feed and backflow material inlet, the benzene of partitioned column side take-off and thiophene cut enter extractive distillation column opening for feed, and tower top is provided with condenser; Extracting rectifying column overhead is provided with refluxing opening, top is provided with extraction agent import, bottom is provided with side line tower gas phase extraction mouth and side line tower liquid-phase reflux mouth, tower top is provided with condenser, reboiler is provided with at the bottom of tower, discharge port at the bottom of tower is connected to tower top extractant feed mouth, and gas phase extraction mouth is connected to side line tower opening for feed; Side line top of tower is provided with refluxing opening, and bottom is provided with gas-phase feed mouth and liquid-phase reflux mouth, and tower top is provided with condenser, and overhead extraction mouth is connected to thick thiophene storage tank; Thick thiophene storage tank is provided with material inlet and outlet, and outlet is connected to thiophene treating tower tower reactor; Be connected with tower reactor bottom thiophene treating tower, top of tower is provided with condenser.
2. device as claimed in claim 1, it is characterized in that being provided with multi-heat exchanger between rough segmentation tower and extractive distillation column, extraction mouth at the bottom of extractive distillation column tower is connected to the import of rough segmentation tower reboiler shell side, be connected to the import of preheater shell side successively, be connected to the import of extractive distillation column feed preheater shell side, finally by being connected to extractive distillation column extractant feed mouth after water cooler.
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| CN104844559A (en) * | 2015-05-21 | 2015-08-19 | 天津大学 | Device and method for extracting thiophene before coking crude benzene hydrogenation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104844559A (en) * | 2015-05-21 | 2015-08-19 | 天津大学 | Device and method for extracting thiophene before coking crude benzene hydrogenation |
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