CN104045506A - Device and process for extracting phenanthrene, fluoranthene and pyrene products in anthracene oil - Google Patents
Device and process for extracting phenanthrene, fluoranthene and pyrene products in anthracene oil Download PDFInfo
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Abstract
The invention belongs to the technical field of advanced treatment of anthracene oil and in particular relates to a device and process for extracting phenanthrene, fluoranthene and pyrene products in anthracene oil. The extracting device comprises an anthracene phenanthrene fraction extraction system and a carbazole fraction extraction system. The extracting device is characterized in that a fluoranthene/pyrene fraction extraction system, a solvent regeneration system, a phenanthrene fraction extraction system and a tail gas purification system are further arranged behind the carbazole fraction extraction system. The extraction device is added with a phenanthrene tower and a fluoranthene/pyrene tower on the previous distillation basis of refined anthracene and carbazole; the setting conditions of the two towers, and the material and filler of the towers are more convenient for extracting the phenanthrene, fluoranthene and pyrene products. The process flow is of four-furnace and four-tower continuous rectification, and capable of producing the anthracene phenanthrene fraction, the carbazole fraction, the fluoranthene fraction, the pyrene fraction and the phenanthrene fraction simultaneously; the process is convenient and flexible to operate, and capable of extracting the phenanthrene, fluoranthene and pyrene having the content of almost 40% in the anthracene oil without increasing more investment; the yield of the products can be more than 80%, and considerable economic benefits can be gained.
Description
Technical field
The invention belongs to carbolineum deep process technology field, especially relate to a kind of carbolineum China and Philippines, fluoranthene, pyrene product extraction element and technique.
Background technology
Coal tar is the byproduct in process of coking, a kind of complex mixture being almost comprised of aromatics completely.In coal tar deep processing process, isolate carbolineum, wherein anthracene, phenanthrene, carbazole, fluoranthene, pyrene are all enriched in carbolineum.Phenanthrene is the aromatic hydrocarbon with three benzene ring structures, the isomers of anthracene.For colourless plate crystal, there is blue-fluorescence, can distil, water insoluble.Luxuriant and rich with fragrance solution has blue-fluorescence, after luxuriant and rich with fragrance conversion processing, can be used for producing dyestuff, medicine and resin etc.; The luxuriant and rich with fragrance perhydro making through hydrogenation is luxuriant and rich with fragrance, can be used for production jet fuel; The luxuriant and rich with fragrance sulfonic acid of sulfonation gained, can be used as binding agent and tanning material.Fluoranthene is a kind of Fourth Ring aromatic hydrocarbons, for yellow-green colour needle crystal, water insoluble, dissolves in dithiocarbonic anhydride and acetic acid, is soluble in ether.Fluoranthene can be used as dyestuff and medical raw material.-8,9 phthaloyl fluoranthene as amino in purple vat dyes 3-, antispasmodic 10b aminoalkyl group-1,2,3 three hydrogen fluoranthene etc.Fluoranthene also can be used as the agent of non-magnetic metal surface inspection.Pyrene is the aromatic hydrocarbon with four benzene ring structures, for the crystallization of faint yellow monocline sheet, water insoluble, is soluble in the organic solvents such as ether and benzene.Pyrene is organic synthesis raw material, through oxidation, can produce Isosorbide-5-Nitrae, and 5,8-naphthalenetetracarbacidic acidic, for dyestuff, synthetic resins, dispersed dyestuff and engineering plastics; Can the gorgeous orange GR of vat dyes processed and other multiple dyestuffs after acidylate; Also can sterilant processed, softening agent etc.Whole world coal tar output is about more than 2,200 ten thousand tons at present, and carbolineum has 5,000,000 tons of left and right at least so, as high value added product phenanthrene, fluoranthene, pyrene in carbolineum, is no less than 180-200 ten thousand tons.
In carbolineum, anthracene, phenanthrene, carbazole, fluoranthene, pyrene are all high boiling point and dystectic aromatics fused ring compound, anthracene content 4.8%-5.5% wherein, carbazole content 2.5%-3.0%, luxuriant and rich with fragrance content 19%-22%, fluoranthene content 9%-11%, pyrene content 6%-8%.In the extraction process that the outer enterprise of Present Domestic provides, just in carbolineum, anthracene, carbazole are extracted, extract total amount and be no more than 6%.The 100000 tons of carbolineums of take are example, I technique: first from carbolineum, crystallization goes out crude anthracene, and then extracts anthracene, carbazole with solvent extration, and output is respectively 1600 tons of anthracenes, carbazole is 600 tons; II technique: be that raw material carries out underpressure distillation with carbolineum, (in the good II technique of extraction effect, anthracene, carbazole sum are 5760 tons, and phenanthrene+fluoranthene+pyrene extracted amount is 26500 tons, accounts for 26.5% of carbolineum total amount to extract respectively 1900 tons of 3860 tons of anthracenes, carbazole.); A large amount of attached value product of height like this is used for making charcoal black, and be the great wasting of resources (price of Vehicles Collected from Market phenanthrene is ten thousand yuan/ton of 2.5-3, and the price of fluoranthene is 5-6 ten thousand yuan/ton, and the price of pyrene is 18.5 ten thousand yuan/ton) real genus.
Summary of the invention
The object of this invention is to provide a kind of carbolineum China and Philippines, fluoranthene, pyrene product extraction element and technique, can from carbolineum, extract in a large number the products such as phenanthrene, fluoranthene, pyrene, reduce cost consumption, realize economic interests and maximize.
The object of the invention is to realize by following technical proposals:
Carbolineum of the present invention is Sino-Philippines, fluoranthene, pyrene product extraction element, comprise the luxuriant and rich with fragrance cut extraction system of anthracene, carbazole cut extraction system, the luxuriant and rich with fragrance cut extraction system of described anthracene comprises the interchanger I connecting successively, interchanger II and interchanger III, the tube furnace I being connected with described interchanger III, the dehydration tower that tube furnace I is connected therewith, the anthracene tower that dehydration tower is connected therewith, be connected to the vapour generator I of this anthracene top of tower, the backflash I that vapour generator I is connected therewith, be connected to the water-and-oil separator at described dehydration tower top, described backflash I is connected with interchanger I, described tube furnace I is connected with described anthracene tower, described anthracene tower side line is connected with described interchanger II,
Described carbazole cut extraction system comprises carbazole cut tower, the tube furnace II that carbazole cut tower is connected therewith, be connected to the vapour generator II of described carbazole fraction overhead portion, the backflash II that vapour generator II is connected therewith, the interchanger IV that backflash II is connected therewith, described carbazole cut tower is connected with described anthracene tower
It is characterized in that being also provided with fluoranthene/pyrene cut extraction system after described carbazole cut extraction system, solvent regeneration system, luxuriant and rich with fragrance cut extraction system and exhaust gas purification system,
Described fluoranthene and pyrene cut extraction system comprise fluoranthene/pyrene tower, the tube furnace III that fluoranthene/pyrene tower is connected therewith, be connected to the vapour generator III of described fluoranthene/pyrene top of tower, the backflash III that vapour generator III is connected therewith, the interchanger V that backflash III is connected therewith, described fluoranthene/pyrene tower is connected with described carbazole cut tower, and described fluoranthene/pyrene tower side line is connected with described interchanger III
Described solvent regeneration system comprises solvent regeneration tower, is connected to dephlegmator and the interchanger VI of this solvent reclamation top of tower, the solvent Receiving bin being connected with described interchanger VI,
Described luxuriant and rich with fragrance cut extraction system comprises luxuriant and rich with fragrance cut tower, the tube furnace IV that luxuriant and rich with fragrance cut tower is connected therewith, be located at the interchanger VIII of described luxuriant and rich with fragrance cut tower side line, be connected to the interchanger VII of described luxuriant and rich with fragrance fraction overhead portion, described interchanger VII is connected with described solvent Receiving bin, described luxuriant and rich with fragrance cut tower is connected with described solvent regeneration tower
Described exhaust gas purification system comprises tail gas purification tower and pump.
Described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and Fei Ta are carbon steel.
Described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and Fei Ta are packing tower.
Described anthracene tower is provided with three opening for feeds and three side line extraction mouths.
An extraction process for carbolineum China and Philippines, fluoranthene, pyrene product, is characterized in that:
(1) standing dehydration carbolineum (water content >=0.5%) is brought up to 180 ℃-190 ℃ through interchanger I, interchanger II and interchanger III carbolineum temperature, entering tube furnace I is heated to 220 ℃ and send above dehydration tower dehydration, anhydrous carbolineum after dehydration enters anthracene tower again after the temperature raising of tube furnace I radiation section, dehydration tower gas phase is brought water and lightweight oil into water-and-oil separator, and separated rear water and lightweight oil flow automatically to respectively storage tank;
(2) the anhydrous carbolineum that enters into anthracene tower carries out decompression separation, top gaseous phase extraction washing oil oil gas enters backflash I after vapour generator I is condensed to 180 ℃, part phegma is returned in anthracene tower, a part enters washing oil storage tank after interchanger I is cooled to 105 ℃, the wash oil fraction of extraction, its main component is naphthalene, acenaphthene, dibenzofuran, fluorenes;
(3) the luxuriant and rich with fragrance cut of anthracene tower side line extraction anthracene, temperature is controlled at 274 ℃-276 ℃, by volume pump, measures after extraction, through interchanger II, be cooled to 140 ℃ to send into below storage tank, as the raw material of producing anthracene, the anthracene content of the luxuriant and rich with fragrance cut of the anthracene herein obtaining is 25-30%, luxuriant and rich with fragrance content 55-60%;
(4) anthracene tower bottoms is the luxuriant and rich with fragrance later component of anthracene, and this part cut regulates through liquid level and flow tandem, and part enters carbazole cut tower, and part is got back to tube furnace I, thermal source is provided to anthracene tower;
(5) carbazole cut tower, gas phase extraction carbazole cut, tower top oil gas is through the cooling laggard backflash II of vapour generator II, part carbazole cut refluxes into carbazole cut tower, a part, through being cooled to 138 ℃-142 ℃, is squeezed into storage tank with pump and is participated in next procedure washing, after washing, is finished product carbazole;
(6) from the side line extraction of carbazole cut tower, being carbon black oil, is viscid bitumen at the bottom of tower, is the raw material of fluoranthene and pyrene, viscid bitumen fluoranthene content >=40% of now extraction, and pyrene content >=30%, pitch composition accounts for 10-12%, and other is for bending and assorted oil distillate;
(7) fluoranthene/pyrene tower, raw material is carbazole cut tower bottoms viscid bitumen, through liquid level and flow tandem, regulate, part viscid bitumen enters fluoranthene/pyrene tower, and part is got back to tube furnace II, thermal source is provided to carbazole cut tower, fluoranthene/pyrene tower bottoms heats by tube furnace III, temperature out is controlled at 370 ℃ of-380 ℃ of left and right and enters fluoranthene/pyrene tower, top gaseous phase extraction fluoranthene cut, and oil gas enters backflash III after vapour generator III is cooling; Part fluoranthene cut refluxes into fluoranthene/pyrene tower, and a part is cooled to 158 ℃-162 ℃ and enters cut storage tank, and as the raw material of producing fluoranthene, fluoranthene/pyrene tower side line extraction pyrene cut, and squeezes into cut storage tank after raw material heat exchange, be the raw material of producing pyrene;
(8) solvent regeneration tower, the anthracene of this technique, carbazole, pyrene all wash with solvent, the anthracene primary crystallization Residual oil of oil-containing solvent oil, carbazole primary crystallization Residual oil and pyrene primary crystallization Residual oil, through interchanger, be heated to 235 ± 3 ℃ of tower middle parts that enter solvent regeneration tower with carbazole column overhead oil gas, fluoranthene/pyrene column overhead oil gas respectively, the solvent oil that tower top is deviate from is cooled to 35 ℃ through dephlegmator, interchanger and enters solvent storage tank, Reusability, solvent regeneration tower tower bottoms, for containing luxuriant and rich with fragrance component, contains luxuriant and rich with fragrance more than 80%;
(9) luxuriant and rich with fragrance cut tower, raw material is containing luxuriant and rich with fragrance component at the bottom of solvent regeneration tower tower, with pump by solvent regeneration tower tower at the bottom of luxuriant and rich with fragrance component send into luxuriant and rich with fragrance cut tower because during solvent regeneration tower extraction solvent, also retain partial solvent in luxuriant and rich with fragrance cut, therefore, luxuriant and rich with fragrance cut column overhead is extraction solvent oil still, cooling rear back dissolving agent receiver, the luxuriant and rich with fragrance cut of luxuriant and rich with fragrance cut tower side line extraction, after heat exchange is cooling, enter luxuriant and rich with fragrance pan tank, then with the crystallization of rotary drum crystallizer, go out qualified phenanthrene;
(10), in this technological process, all production equipments, storage tank etc. enter tail gas purification tower and carry out tail gas clean-up recovery.
Described anthracene column overhead pressure-controlling is at 10-15KPa, and temperature is controlled at 230 ± 2 ℃; Anthracene tower tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 326 ± 2 ℃.Tube furnace I outlet hot oil temperature is controlled at 350-355 ℃.
Described carbazole cut column overhead pressure-controlling is at 10 ± 2KPa, and temperature is controlled at 290 ℃ ± 2 ℃; Tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 330 ℃ ± 2.
Described fluoranthene/pyrene column overhead pressure-controlling is at 15 ± 2KPa, and tower top temperature is controlled at 325 ± 2 ℃, and tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 360-365 ℃.
In described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and luxuriant and rich with fragrance cut tower, negative-pressure vacuum degree is >=-85Kpa.
Advantage of the present invention:
(1) carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and technique, on the distillation basis of former anthracene, carbazole, luxuriant and rich with fragrance tower and fluoranthene, pyrene tower have been increased, the be more convenient for extraction of phenanthrene, fluoranthene, pyrene product of the condition that arranges of these two towers, the material of tower and filler.Four stove four tower continuous rectifications are taked in technical process of the present invention, produce the luxuriant and rich with fragrance oil of anthracene, carbazole fraction, fluoranthene fraction simultaneously, pyrene fraction, easy to operate, flexible, in the situation that not increasing more investments, the phenanthrene, fluoranthene, the pyrene that account for content nearly 40% in carbolineum are extracted, and yield can reach more than 80%, can obtain considerable economic benefit;
(2) the present invention extracts from carbolineum phenanthrene, fluoranthene, pyrene adopt short flow process, and luxuriant and rich with fragrance raw material sources, in solvent recuperation tower reactor, directly enter luxuriant and rich with fragrance tower with recycle pump; The raw material sources of fluoranthene and pyrene, in carbazole cut tower tower reactor, are also directly to enter fluoranthene and pyrene tower with pump, and top gaseous phase is fluoranthene, side line liquid phase extraction pyrene.Adopt short flow process, mainly solved the physical property that pyrene can not heat repeatedly, thoroughly solved material coking problem; Abbreviated system has also significantly reduced gas consumption, has avoided the drawback of raw material normal temperature heating temperature raising, has reduced a large amount of support equipments, as storage tank, medial launder, interchanger etc. simultaneously; Because of short flow process, 3 products adopt 2 towers, than routine distillation, have saved a tower, and two king-towers are taked the type of heating of pump circulation, whole system utilizes product and intermediates to conservation measuress such as raw material preheatings simultaneously, and system energy consumption is low, and energy consumption is 75% left and right with scale systems;
(3) carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and process using underpressure distillation, this underpressure distillation condition requires high than common underpressure distillation, boiling point and fusing point for phenanthrene, fluoranthene, pyrene, negative-pressure vacuum degree must guarantee-more than 85KPa, tower reactor and tower top temperature must be controlled at specified temperature ± 2 ℃, adopt sub-pressure high-efficient rectifying, reduced rectification temperature, prevent high-temperature coking;
(4) in carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and technique, the requirement of vacuum tightness is very high, for fear of sublimate, sucks vacuum pipe, adopts double-condenser, and increases nitrogen purging, efficiently solves the blockage problem of vacuum pipe;
(5) quality index of carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and technique China and Philippines, fluoranthene, pyrene all can reach more than 98%, and particularly luxuriant and rich with fragrance, fluoranthene does not need with solvent wash, direct crystallization;
(6) in carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and technique, anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and Fei Ta are packing tower, guarantee separating effect, have saved investment.
Accompanying drawing explanation
Fig. 1 is distil process schema of the present invention.
Fig. 2 is washing process schema of the present invention.
Embodiment
Below in conjunction with accompanying drawing, further illustrate the specific embodiment of the present invention.
As shown in Figure 1, carbolineum of the present invention is Sino-Philippines, fluoranthene, pyrene product extraction element, comprise the luxuriant and rich with fragrance cut extraction system of anthracene, carbazole cut extraction system, the luxuriant and rich with fragrance cut extraction system of described anthracene comprises the interchanger I 1 connecting successively, interchanger II 2 and interchanger III 3, the tube furnace I 6 being connected with described interchanger III 3, the dehydration tower 5 that tube furnace I 6 is connected therewith, the anthracene tower 7 that dehydration tower 5 is connected therewith, be connected to the vapour generator I 8 at these anthracene tower 7 tops, the backflash I 9 that vapour generator I 8 is connected therewith, be connected to the water-and-oil separator 4 at described dehydration tower 5 tops, described backflash I 9 is connected with interchanger I 1, described tube furnace I 6 is connected with described anthracene tower 7, described anthracene tower 7 side lines are connected with described interchanger II 2,
Described carbazole cut extraction system comprises carbazole cut tower 11, the tube furnace II 10 that carbazole cut tower 11 is connected therewith, be connected to the vapour generator II 12 at described carbazole cut tower 11 tops, the backflash II 14 that vapour generator II 12 is connected therewith, the interchanger IV 13 that backflash II 14 is connected therewith, described carbazole cut tower 11 is connected with described anthracene tower 7
It is characterized in that being also provided with fluoranthene/pyrene cut extraction system after described carbazole cut extraction system, solvent regeneration system, luxuriant and rich with fragrance cut extraction system and exhaust gas purification system,
Described fluoranthene and pyrene cut extraction system comprise fluoranthene/pyrene tower 16, the tube furnace III 15 that fluoranthene/pyrene tower 16 is connected therewith, be connected to the vapour generator III 17 at described fluoranthene/pyrene tower 16 tops, the backflash III 19 that vapour generator III 17 is connected therewith, the interchanger V 18 that backflash III 19 is connected therewith, described fluoranthene/pyrene tower 16 is connected with described carbazole cut tower 11, and described fluoranthene/pyrene tower 16 side lines are connected with described interchanger III 3
Described solvent regeneration system comprises solvent regeneration tower 20, is connected to dephlegmator and the interchanger VI 21 at these solvent regeneration tower 20 tops, the solvent Receiving bin 22 being connected with described interchanger VI 21,
Described luxuriant and rich with fragrance cut extraction system comprises luxuriant and rich with fragrance cut tower 24, the tube furnace IV 23 that luxuriant and rich with fragrance cut tower 24 is connected therewith, be located at the interchanger VIII 25 of described luxuriant and rich with fragrance cut tower 24 side lines, be connected to the interchanger VII 26 at described luxuriant and rich with fragrance cut tower 24 tops, described interchanger VII 26 is connected with described solvent Receiving bin 22, described luxuriant and rich with fragrance cut tower 24 is connected with described solvent regeneration tower 20
Described exhaust gas purification system comprises tail gas purification tower 27 and pump 28.
Described anthracene tower 7, carbazole cut tower 11, fluoranthene/pyrene tower 16 and Fei Ta 24 are carbon steel.
Described anthracene tower 7, carbazole cut tower 34, fluoranthene/pyrene tower 16 and Fei Ta 24 are packing tower.
Described anthracene tower 7 is provided with three opening for feeds and three side line extraction mouths.
An extraction process for carbolineum China and Philippines, fluoranthene, pyrene product, is characterized in that adopting four stove four tower negative pressure rectification process, separated through four towers, obtains the luxuriant and rich with fragrance oil of anthracene, carbazole fraction, fluoranthene and pyrene cut.
One, carbolineum distillation system
(1) get in the carbolineum of standing dehydration and crude anthracene mixing oil (water content ≯ 0.5%) Yong Bengcongcao district, through interchanger I 1, interchanger II 2, interchanger III 3(interchanger I 1 is raw material/washing oil interchanger, interchanger II 2 is the luxuriant and rich with fragrance cut interchanger of raw material/anthracene, interchanger III 3 is raw material/viscid bitumen interchanger) behind heat exchange to 180～190 ℃, after being heated to 210～220 ℃, tube furnace I 6 convection zones send dehydration tower 5 again, by efficient traverse baffle flash distillation, deviate from moisture wherein to slow down the corrosion of follow-up equipment, dehydration tower 5 head temperature control to 170～180 ℃, tower reactor temperature controls to 200～210 ℃, anhydrous heavy oil fraction after dehydration is moisture is less than 0.08%, after being regulated by dehydration tower 5 tower reactor liquid levels and flow tandem, be sent to anthracene tower 7.Dehydration tower 5 tower top oil gas enter after water-and-oil separator 4 separation after being condensed to 50 ℃, and waste water is to wastewater trough, and light oil is to washing oil groove;
(2) the anthracene cut after dehydration is in anthracene tower 7 decompression separation, top of tower washing oil oil gas out enters backflash I 9 after vapour generator I 8 is condensed to 180 ℃, part liquid is returned in anthracene tower 7 circulation by backflash I 9 through reflux pump, and a part is regulated by backflash I 9 liquid levels and interchanger I 1 enters washing oil fraction medial launder to 105 ℃ after cooling.The washing oil fraction major ingredient of extraction is naphthalene, acenaphthene, dibenzofuran, fluorenes;
(3) the luxuriant and rich with fragrance cut of anthracene tower 7 side line extraction anthracenes, temperature is controlled at 274 ℃-276 ℃, by volume pump, measures after extraction, through interchanger II 2, be cooled to 140 ℃ to send into below storage tank, as the raw material of producing anthracene, the anthracene content of the luxuriant and rich with fragrance cut of the anthracene herein obtaining is 25-30%, luxuriant and rich with fragrance content 55-60%; This technique is considered diversity and the unstable of raw material, and anthracene tower 7 is provided with three opening for feeds and three side line extraction mouths;
(4) anthracene tower 7 bottomss are the luxuriant and rich with fragrance later component of anthracene, and this part cut regulates through liquid level and flow tandem, and part enters carbazole cut tower 11, and part is got back to tube furnace I 6, thermal source are provided to anthracene tower 7; For slowing down coking and the polymerization of heavy constituent in rectifying, anthracene tower 7 adopts rectification under vacuum.The gas phase of the washing oil fraction that tower top is overflowed is after vapour generator I 8, and liquid phase enters return-flow system, and the non-condensable gas of condensate cooler connects vacuum system.Anthracene tower 7 tower top pressures are controlled at 10-15KPa, and temperature is controlled at 230 ± 2 ℃; Anthracene tower 7 tower bottom pressures are controlled at 20-30KPa, and temperature is controlled at 326 ± 2 ℃.Tower reactor heat provides by tube furnace I heated by gas, and tube furnace I 6 thermal loads are 4,500,000 kcal/h, tube furnace I 6 outlet hot oil temperature 350-355 ℃;
(5) carbazole cut tower 11, gas phase extraction carbazole cut, tower top oil gas is through the cooling laggard backflash II 14 of vapour generator II 12, part carbazole cut refluxes into carbazole cut tower 11, a part is through being cooled to 138 ℃-142 ℃, with pump, squeezing into storage tank and participate in next procedure washing, is finished product carbazole after washing;
At carbazole cut tower 11 tower top oil gas, through vapour generator II 12, being condensed to 234 ± 3 ℃ and non-condensable gases condensation is cooled to 50 ℃ of left and right and enters vacuum system.The pressure-controlling of tower top is at 10 ± 2KPa, and temperature is controlled at 290 ± 2 ℃; Tower bottom pressure is controlled at 20～30KPa, and temperature is controlled at 330 ℃ ± 2 ℃;
In order further to reduce system energy consumption, still carbazole cut tower 11 tower top oil gas and the heat exchange of solvent regeneration system regeneration Residual oil have been reserved, from the oil gas and the heat exchange of anthracene/carbazole/pyrene primary crystallization Residual oil of 290 ± 2 ℃ of the temperature of overhead extraction, then enter vapour generator II 12;
(6) to be reserved with extraction major ingredient be carbon black oil cut side line to carbazole cut tower 11 stripping sections, this fraction is got by pump, part through with raw material heat exchange after, through cooling inflow carbon black oil cut storage tank, be used for preparing carbon black oil or as the raw material of carbolineum hydrogenation, tower reactor is returned to carbazole cut tower 11 after partly entering 10 heating of tube furnace II, thermal source is provided to carbazole cut tower 11.Tower reactor fluxed bitumen (mainly containing fluoranthene, pyrene) is got by recycle pump, and part enters fluoranthene/pyrene tower 16 through liquid level and the adjusting of flow tandem, and part enters 10 heating of tube furnace II, thermal source is provided to carbazole cut tower 11;
(7) fluoranthene/pyrene tower 16 tower top fluoranthene oil gas are condensed to 170 ± 3 ℃ of left and right through vapour generator III 17 and enter backflash III 19, and part is returned stream, and part enters fluoranthene storage tank after heat exchange is cooling.Non-condensable gases condensate cooler is cooled to 50 ℃ of left and right and enters vacuum system.The pressure-controlling of fluoranthene/pyrene tower 16 tower tops is at 15 ± 2KPa, and temperature is controlled at 325 ± 2 ℃ of left and right; Tower bottom pressure is controlled at 20～30KPa, and temperature is controlled at 360～365 ℃ of left and right, and tower reactor heat provides by tube furnace III 15 heated by gas, and tube furnace III 15 thermal loads are 2,400,000 kcal/h, tube furnace III 15 outlet 375～385 ℃ of left and right of hot oil temperature;
It is pyrene side line that fluoranthene/pyrene tower 16 stripping sections are reserved with extraction major ingredient, this fraction is got by pump, part through with raw material heat exchange after, through cooling inflow pyrene cut storage tank, be used as the raw material of producing pyrene, tower reactor is returned to fluoranthene/pyrene tower 16 after partly entering 15 heating of tube furnace III, thermal source is provided to fluoranthene/pyrene tower 16.Part regulates and enters carbon black oil groove through liquid level and flow tandem, with the heavy wash oil cut of the anthracene tower 7 tower tops carbon black oil that is mixed;
Two, solvent regeneration system
(8) the anthracene primary crystallization Residual oil of oil-containing solvent oil, carbazole primary crystallization Residual oil and pyrene primary crystallization Residual oil are heated to 235 ± 3 ℃ of tower middle parts that enter solvent regeneration tower 20 with carbazole tower 11 tower top oil gas, fluoranthene/pyrene tower 16 tower top oil gas, fluoranthene/pyrene tower 16 tower reactor viscid bitumens through interchanger respectively, tower top is deviate from 75% solvent oil oil gas through dephlegmator partial reflux, after gas phase and the heat exchange of regeneration Residual oil, water at low temperature is cooled to 35 ± 3 ℃ to enter regenerated solvent Receiving bin 22.Solvent regeneration tower 20 tower reactor medium liquid levels and flow tandem are sent into luxuriant and rich with fragrance cut tower 24 middle parts (Residual oil of anthracene primary crystallization) after regulating, as producing the luxuriant and rich with fragrance raw material of essence; In order to guarantee regeneration efficiency, regeneration adopts negative pressure, and solvent regeneration tower 20 tower top pressures are controlled at 20 ± 3KPa, and tower bottom pressure is controlled at 35～50Kpa; Solvent regeneration tower tower bottoms, for containing luxuriant and rich with fragrance component, contains luxuriant and rich with fragrance more than 80%;
(9) luxuriant and rich with fragrance cut tower 24, raw material is containing luxuriant and rich with fragrance component at the bottom of solvent regeneration tower 20 towers, with pump by solvent regeneration tower 20 towers at the bottom of luxuriant and rich with fragrance component send into luxuriant and rich with fragrance cut tower 24 because during solvent regeneration tower 20 extraction solvent, also retain partial solvent in luxuriant and rich with fragrance cut, therefore, luxuriant and rich with fragrance cut tower 24 tower tops are extraction solvent oil still, cooling rear back dissolving agent Receiving bin 22, the luxuriant and rich with fragrance cut of luxuriant and rich with fragrance cut tower 24 side line extraction, after heat exchange is cooling, enter luxuriant and rich with fragrance pan tank, then with the crystallization of rotary drum crystallizer, go out qualified phenanthrene; The pressure-controlling of luxuriant and rich with fragrance cut tower 24 tower tops is at 20 ± 3KPa, and temperature is controlled at 280 ± 3 ℃ of left and right; Tower bottom pressure is controlled at 30～50KPa, and temperature is controlled at 310～315 ℃ of left and right; Tower reactor is returned to luxuriant and rich with fragrance cut tower 24 after partly entering 23 heating of tube furnace IV, thermal source is provided to luxuriant and rich with fragrance cut tower 24.Part regulates and enters carbon black oil groove through liquid level and flow tandem, with the heavy wash oil cut of the anthracene tower 7 tower tops carbon black oil that is mixed;
(10), in this technological process, the tail gas of the generations such as all production equipments, storage tank enters tail gas purification tower 27 and carries out tail gas clean-up recovery.
In the process engineering of the present invention's four stove four column distillations, anthracene tower 7, carbazole cut tower 11, fluoranthene/pyrene tower 16 and the interior negative-pressure vacuum degree of luxuriant and rich with fragrance cut tower 24 are >=-85Kpa.
Three, washing dehumidification system
As shown in Figure 2, the carbazole/anthracene/pyrene cut extracting in carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction process need to be through washing, dehumidification system purify out carbazole, anthracene and pyrene finished product.Carbazole/anthracene/pyrene cut is mixed after groove 29 mixes and is pumped into 30 washings of carbazole/anthracene/pyrene cut washing filter by transferpump through carbazole/anthracene/pyrene cut together with solvent, 31 vacuum-dryings of carbazole/anthracene after washing/pyrene cut drying machine, obtain carbazole, anthracene and pyrene finished product, through carbazole/anthracene/pyrene cut washing filter 30 crystallization Residual oil out, enter Residual oil Receiving bin 32.Fluoranthene/luxuriant and rich with fragrance cut, without the washing of washing dehumidification system, can obtain fluoranthene, luxuriant and rich with fragrance finished product through high the putting after groove 33 enters 34 crystallizations of rotary drum crystallizer of fluoranthene/luxuriant and rich with fragrance cut.
Each shell and tube cooler backwater of the present invention returns water cooling tower after concentrating and entering recirculated water backwater water-main, in water cooling tower, be uniformly distributed the air cooling that the circulating hot water of whereabouts is risen, drop to flow automatically to behind pond and in pond, complete circulation, cooled water is again recycled water pump extraction and is sent to each water cooler, thereby completes whole closed cycle.Technique vacuum of the present invention is had relatively high expectations, drawback is that sublimate sucks vacuum pipe, for head it off, can adopt double-condenser measure at gas phase and the liquid phase production end of anthracene tower 7, carbazole cut tower 11, fluoranthene/pyrene tower 16 and Fei Ta 24, and increasing nitrogen purging, the problem of the stifled vacuum pipe occurring in technique can solve completely.
Four stove four tower continuous rectifications are taked in equipment of the present invention and technical process, produce the luxuriant and rich with fragrance oil of anthracene, carbazole fraction, fluoranthene fraction simultaneously, pyrene fraction, easy to operate, flexible, in the situation that not increasing more investments, the phenanthrene, fluoranthene, the pyrene that account for content nearly 40% in carbolineum are extracted, and yield can reach more than 80%, can obtain considerable economic benefit.In technique, adopt short flow process, mainly solved the physical property that pyrene can not heat repeatedly, thoroughly solved material coking problem.Abbreviated system has also significantly reduced gas consumption, has avoided the drawback of raw material normal temperature heating temperature raising, has reduced a large amount of support equipments, as storage tank, medial launder, interchanger etc. simultaneously.Because of short flow process, 3 products adopt 2 towers, than routine distillation, have saved a tower, and meanwhile, whole system utilizes product and intermediates to conservation measuress such as raw material preheatings, and system energy consumption is low, and energy consumption is 75% left and right with scale systems.
Extraction through technique of the present invention to carbolineum China and Philippines, fluoranthene, pyrene product, the quality index of phenanthrene, fluoranthene, pyrene all can reach more than 98%, and particularly luxuriant and rich with fragrance, fluoranthene does not need with solvent wash, direct crystallization.
Carbolineum of the present invention China and Philippines, fluoranthene, pyrene product extraction element and technology investment are little, and output is high, and has improved the purification precision to phenanthrene, fluoranthene, pyrene product, are applicable to extensively promoting and using.
Claims (9)
1. carbolineum China and Philippines, fluoranthene, pyrene product extraction element, comprise the luxuriant and rich with fragrance cut extraction system of anthracene, carbazole cut extraction system, the luxuriant and rich with fragrance cut extraction system of described anthracene comprises the interchanger I connecting successively, interchanger II and interchanger III, the tube furnace I being connected with described interchanger III, the dehydration tower that tube furnace I is connected therewith, the anthracene tower that dehydration tower is connected therewith, be connected to the vapour generator I of this anthracene top of tower, the backflash I that vapour generator I is connected therewith, be connected to the water-and-oil separator at described dehydration tower top, described backflash I is connected with interchanger I, described tube furnace I is connected with described anthracene tower, described anthracene tower side line is connected with described interchanger II,
Described carbazole cut extraction system comprises carbazole cut tower, the tube furnace II that carbazole cut tower is connected therewith, be connected to the vapour generator II of described carbazole fraction overhead portion, the backflash II that vapour generator II is connected therewith, the interchanger IV that backflash II is connected therewith, described carbazole cut tower is connected with described anthracene tower
It is characterized in that being also provided with fluoranthene/pyrene cut extraction system after described carbazole cut extraction system, solvent regeneration system, luxuriant and rich with fragrance cut extraction system and exhaust gas purification system,
Described fluoranthene and pyrene cut extraction system comprise fluoranthene/pyrene tower, the tube furnace III that fluoranthene/pyrene tower is connected therewith, be connected to the vapour generator III of described fluoranthene/pyrene top of tower, the backflash III that vapour generator III is connected therewith, the interchanger V that backflash III is connected therewith, described fluoranthene/pyrene tower is connected with described carbazole cut tower, and described fluoranthene/pyrene tower side line is connected with described interchanger III
Described solvent regeneration system comprises solvent regeneration tower, is connected to dephlegmator and the interchanger VI of this solvent reclamation top of tower, the solvent Receiving bin being connected with described interchanger VI,
Described luxuriant and rich with fragrance cut extraction system comprises luxuriant and rich with fragrance cut tower, the tube furnace IV that luxuriant and rich with fragrance cut tower is connected therewith, be located at the interchanger VIII of described luxuriant and rich with fragrance cut tower side line, be connected to the interchanger VII of described luxuriant and rich with fragrance fraction overhead portion, described interchanger VII is connected with described solvent Receiving bin, described luxuriant and rich with fragrance cut tower is connected with described solvent regeneration tower
Described exhaust gas purification system comprises tail gas purification tower and pump.
2. carbolineum according to claim 1 China and Philippines, fluoranthene, pyrene product extraction element, is characterized in that described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and Fei Ta are carbon steel.
3. carbolineum according to claim 1 China and Philippines, fluoranthene, pyrene product extraction element, is characterized in that described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and Fei Ta are packing tower.
4. according to the carbolineum China and Philippines described in claim 1,2 or 3, fluoranthene, pyrene product extraction element, it is characterized in that described anthracene tower is provided with three opening for feeds and three side line extraction mouths.
5. an extraction process for carbolineum China and Philippines, fluoranthene, pyrene product, is characterized in that:
(1) standing dehydration carbolineum (water content >=0.5%) is brought up to 180 ℃-190 ℃ through interchanger I, interchanger II and interchanger III carbolineum temperature, entering tube furnace I is heated to 220 ℃ and send above dehydration tower dehydration, anhydrous carbolineum after dehydration enters anthracene tower again after the temperature raising of tube furnace I radiation section, dehydration tower gas phase is brought water and lightweight oil into water-and-oil separator, and separated rear water and lightweight oil flow automatically to respectively storage tank;
(2) the anhydrous carbolineum that enters into anthracene tower carries out decompression separation, top gaseous phase extraction washing oil oil gas enters backflash I after vapour generator I is condensed to 180 ℃, part phegma is returned in anthracene tower, a part enters washing oil storage tank after interchanger I is cooled to 105 ℃, the wash oil fraction of extraction, its main component is naphthalene, acenaphthene, dibenzofuran, fluorenes;
(3) the luxuriant and rich with fragrance cut of anthracene tower side line extraction anthracene, temperature is controlled at 274 ℃-276 ℃, by volume pump, measures after extraction, through interchanger II, be cooled to 140 ℃ to send into below storage tank, as the raw material of producing anthracene, the anthracene content of the luxuriant and rich with fragrance cut of the anthracene herein obtaining is 25-30%, luxuriant and rich with fragrance content 55-60%;
(4) anthracene tower bottoms is the luxuriant and rich with fragrance later component of anthracene, and this part cut regulates through liquid level and flow tandem, and part enters carbazole cut tower, and part is got back to tube furnace I, thermal source is provided to anthracene tower;
(5) carbazole cut tower, gas phase extraction carbazole cut, tower top oil gas is through the cooling laggard backflash II of vapour generator II, part carbazole cut refluxes into carbazole cut tower, a part, through being cooled to 138 ℃-142 ℃, is squeezed into storage tank with pump and is participated in next procedure washing, after washing, is finished product carbazole;
(6) from the side line extraction of carbazole cut tower, being carbon black oil, is viscid bitumen at the bottom of tower, is the raw material of fluoranthene and pyrene, viscid bitumen fluoranthene content >=40% of now extraction, and pyrene content >=30%, pitch composition accounts for 10-12%, and other is for bending and assorted oil distillate;
(7) fluoranthene/pyrene tower, raw material is carbazole cut tower bottoms viscid bitumen, through liquid level and flow tandem, regulate, part viscid bitumen enters fluoranthene/pyrene tower, and part is got back to tube furnace II, thermal source is provided to carbazole cut tower, fluoranthene/pyrene tower bottoms heats by tube furnace III, temperature out is controlled at 370 ℃ of-380 ℃ of left and right and enters fluoranthene/pyrene tower, top gaseous phase extraction fluoranthene cut, and oil gas enters backflash III after vapour generator III is cooling; Part fluoranthene cut refluxes into fluoranthene/pyrene tower, and a part is cooled to 158 ℃-162 ℃ and enters cut storage tank, and as the raw material of producing fluoranthene, fluoranthene/pyrene tower side line extraction pyrene cut, and squeezes into cut storage tank after raw material heat exchange, be the raw material of producing pyrene;
(8) solvent regeneration tower, the anthracene of this technique, carbazole, pyrene all wash with solvent, the anthracene primary crystallization Residual oil of oil-containing solvent oil, carbazole primary crystallization Residual oil and pyrene primary crystallization Residual oil, through interchanger, be heated to 235 ± 3 ℃ of tower middle parts that enter solvent regeneration tower with carbazole column overhead oil gas, fluoranthene/pyrene column overhead oil gas respectively, the solvent oil that tower top is deviate from is cooled to 35 ℃ through dephlegmator, interchanger and enters solvent storage tank, Reusability, solvent regeneration tower tower bottoms, for containing luxuriant and rich with fragrance component, contains luxuriant and rich with fragrance more than 80%;
(9) luxuriant and rich with fragrance cut tower, raw material is containing luxuriant and rich with fragrance component at the bottom of solvent regeneration tower tower, with pump by solvent regeneration tower tower at the bottom of luxuriant and rich with fragrance component send into luxuriant and rich with fragrance cut tower because during solvent regeneration tower extraction solvent, also retain partial solvent in luxuriant and rich with fragrance cut, therefore, luxuriant and rich with fragrance cut column overhead is extraction solvent oil still, cooling rear back dissolving agent receiver, the luxuriant and rich with fragrance cut of luxuriant and rich with fragrance cut tower side line extraction, after heat exchange is cooling, enter luxuriant and rich with fragrance pan tank, then with the crystallization of rotary drum crystallizer, go out qualified phenanthrene;
(10), in this technological process, all production equipments, storage tank etc. enter tail gas purification tower and carry out tail gas clean-up recovery.
6. the extraction process of a kind of carbolineum according to claim 5 China and Philippines, fluoranthene, pyrene product, is characterized in that described anthracene column overhead pressure-controlling is at 10-15KPa, and temperature is controlled at 230 ± 2 ℃; Anthracene tower tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 326 ± 2 ℃,
Tube furnace I outlet hot oil temperature is controlled at 350-355 ℃.
7. the extraction process of a kind of carbolineum according to claim 5 China and Philippines, fluoranthene, pyrene product, is characterized in that described carbazole cut column overhead pressure-controlling is at 10 ± 2KPa, and temperature is controlled at 290 ℃ ± 2 ℃; Tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 330 ℃ ± 2.
8. the extraction process of a kind of carbolineum China and Philippines according to claim 5,, fluoranthene, pyrene product, it is characterized in that described fluoranthene/pyrene column overhead pressure-controlling is at 15 ± 2KPa, tower top temperature is controlled at 325 ± 2 ℃, and tower bottom pressure is controlled at 20-30KPa, and temperature is controlled at 360-365 ℃.
9. the extraction process of a kind of carbolineum according to claim 5 China and Philippines, fluoranthene, pyrene product, is characterized in that in described anthracene tower, carbazole cut tower, fluoranthene/pyrene tower and luxuriant and rich with fragrance cut tower that negative-pressure vacuum degree is for >=-85Kpa.
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