CN105713647A - Method and device for maximally preparing phenol-containing oil and diesel oil from coal tar - Google Patents
Method and device for maximally preparing phenol-containing oil and diesel oil from coal tar Download PDFInfo
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- CN105713647A CN105713647A CN201610200901.4A CN201610200901A CN105713647A CN 105713647 A CN105713647 A CN 105713647A CN 201610200901 A CN201610200901 A CN 201610200901A CN 105713647 A CN105713647 A CN 105713647A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/06—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by heating, cooling, or pressure treatment
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
Abstract
The invention provides a method and a device for maximally preparing phenol-containing oil and diesel oil from coal tar. The method comprises steps as follows: coal tar is subjected to flash evaporation treatment, obtained flash evaporation oil is subjected to delayed coking, and oil gas and pitch coke are prepared; flash evaporation gas and oil gas are subjected to fractional distillation together, and crude gasoline, overhead cycle oil, crude diesel oil and tail oil are obtained; the crude gasoline is separated, and stable gasoline is prepared and mixed with the overhead cycle oil to be used as the phenol-containing oil; the crude diesel oil is subjected to hydrotreatment, and refined diesel oil and naphtha are obtained. With the adoption of the method, the crude gasoline is separated initiatively, the stable gasoline is obtained and mixed with the overhead cycle oil to be used as the phenol-containing oil, compared with an existing technology for preparing crude phenol from coal tar, the method has the advantages that the crude gasoline approximately accounting for 40wt% of the total amount of the phenol-containing oil in the coal tar is properly treated to be used as the phenol-containing oil, and the yield of the phenol-containing oil is greatly increased, so that the yield of the phenol-containing oil prepared from the coal tar is maximized.
Description
Technical field
The present invention relates to coal tar processing technology field, particularly relate to a kind of method utilizing coal tar maximization to prepare carbolic oil and diesel oil and device.
Background technology
China is oil product consumption big country, but is again that petroleum resources are poor and the country of coal resources relative abundance simultaneously.Along with the day by day exhausted of petroleum resources and being growing on and on to demand for energy, the price of some chemical products obtained by petrochemical industry rises suddenly, and these chemical products also are able to from coal gasification equally, the products such as dry distilling directly or indirectly obtain, hence with advanced coal conversion technology development Modern Coal-based Chemical, produce gasoline, diesel oil and chemical products, the not only industry restructuring to chemical industry, lifting industry energy level has the effect of actively promoting, 21 century alleviates China to petroleum import interdependency especially, develop a circular economy, reduce environmental pollution, ensure the strategic measure of Chinese energy safety and sustainable economic development.
The tar containing fine coal be fine coal carbonization at 350～700 DEG C obtain a kind of in black or the thick fluid product of pitchy, its composition is extremely complex, may separate out multiple product.Phenolic compound contained in coal tar is current comparatively important high value added product and industrial chemicals, and it has purposes widely in synthetic fibers, engineering plastics, pesticide, medicine, explosive, plasticizer, preservative, spice and fuel intermediate etc..In coal tar, the productivity of aldehydes matter is limited mainly by ature of coal and the impact of Coal Chemical Industry process conditions, and in general, in low temperature pyrogenation product, the mass fraction of phenolic compound is about 20%～30%.Therefore, from coal tar, extract aldehydes matter, not only there is good economic benefit, obtain higher profit for enterprise, be also equipped with certain social benefit and environmental benefit simultaneously, protect periphery ecological environment.
At present, the method extracting crude phenols from coal tar mainly has washing method, extraction, settling methods and rectification method etc., and these processing methods simply simply extract crude phenols from coal tar, and the working depth of coal tar is inadequate, and overall economic benefit is not high.For overcoming this technological deficiency, Chinese patent literature 103450939A discloses a kind of method that middle coalite tar delayed coking unit extracts crude phenols, comprise the following steps: first middle coalite tar heat exchange is entered coal tar stripper after 260～300 DEG C, coal tar is partitioned into stripper top gas and heavy distillat in stripper, and stripper top gas enters fractionating column secondary separation；Heavy distillat and recycle oil are mixed into heating furnace and are warming up to 400～500 DEG C, then enter back into coke drum, carry out cracking and condensation reaction in coke drum, generate oil gas and pitch coke；Then oil gas is sent into fractionating column and carries out product separation, fractionate out rich gas, gasoline, carbolic oil, diesel oil, wax oil and cycle oil fraction from top to bottom；Carbolic oil is carried out phenol removal, obtains crude phenols and dephenolize oil；Finally gasoline, dephenolize oil, diesel oil, wax oil are carried out hydrotreatment, prepare hydrotreated naphtha and hydrogenated diesel oil.
Although middle coalite tar can be changed into light diesel, Petroleum and petroleum coke by above-mentioned technology, extract the crude phenols oil obtaining having high added value simultaneously, but the gasoline accounting for carbolic oil total amount 40wt% in coal tar is made directly hydrotreatment to prepare the relatively low diesel oil of price and Petroleum by this technology, without carrying out rationally effective processing and utilization, this reduces the yield of carbolic oil undoubtedly, reduce the economic benefit of whole technique, cause the huge wasting of resources.Additionally, due to containing fine coal tar contains the coke powder of more amount, coal dust, above-mentioned technology process unit when processing containing fine coal tar is made to be prone to coking, it is difficult to long-term operation continuously and stably, that is to say, the prior art is bigger to the limitation of raw materials technology, it is impossible to process rising pulverized coal pyrolysis field containing fine coal tar.Therefore, how to improve to overcome above-mentioned deficiency to the method for existing middle coalite tar crude phenols, be this area technical barrier urgently to be resolved hurrily.
Summary of the invention
Present invention solves the technical problem that the defect being in that to overcome the carbolic oil yield existing for existing coal tar crude phenols technology low, and then a kind of method utilizing coal tar maximization to prepare carbolic oil and diesel oil and device are provided.
Another technical problem that this invention address that is in that the defect containing fine coal tar that cannot process overcome existing for existing coal tar crude phenols technology, and then provides a kind of method and device to prepare carbolic oil and diesel oil for raw material maximization containing fine coal tar.
For this, the present invention realizes the technical scheme of above-mentioned purpose and is:
A kind of method utilizing coal tar maximization to prepare carbolic oil and diesel oil, including:
(1) coal tar is carried out flash distillation process, collect the flashed vapour and flash oil that obtain respectively；
(2) described flash oil is carried out delayed coking, obtain oil gas and pitch coke；
(3) described oil gas and described flashed vapour are carried out fractional distillation process jointly, obtain raw gasoline, top recycle oil, gas-oil and tail oil；
(4) described raw gasoline is easily separated process and obtains stable gasoline removing light hydrocarbon, described stable gasoline is merged as carbolic oil with described top recycle oil；
(5) described gas-oil is carried out hydrotreatment, obtain refined diesel oil and Petroleum.
Described coal tar be containing 1-10wt% dust containing fine coal tar, described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
In step (1), after described coal tar is preheated to 260-320 DEG C, it is mixed to form miscella with the described tail oil of part, described miscella is carried out described flash distillation process.
In step (2), described delayed coking is to carry out when 420-490 DEG C, 0.1-0.3MPa and recycle ratio are 0.3-0.8.
In step (3), carry out three phase separation after described fractional distillation is processed the gas phase cooling obtained, respectively obtain rich gas, sour water and described raw gasoline.
The sweet gas that described rich gas obtains after desulfurization is for heating described coal tar and/or described flash oil.
Described sour water is carried out stripping process, obtains thick ammonia and sour gas；Described thick ammonia obtains liquefied ammonia after ammonia refining, and described sour gas obtains sulfur after Cross unit processes.
In step (4), the heating of described raw gasoline is easily separated process to entering in stabilizer after 100-130 DEG C；Described light hydrocarbon cooled post liquefaction part returns in described stabilizer as overhead reflux, and another part mixes with described gas-oil and carries out described hydrotreatment.
A kind of device utilizing coal tar maximization to prepare carbolic oil and diesel oil, including:
Flash column, is provided with raw oil import, flashed vapour outlet and flash oil outlet；
Coke drum, its import is connected setting with the outlet of described flash oil, and described coke drum is provided with pitch coke outlet and oil gas vent；
Connecting, with the outlet of described flashed vapour and described oil gas vent, the fractionating column arranged respectively, described fractionating column is provided with gaseous phase outlet, top recycle oil outlet and gas-oil outlet；
Stabilizer, its import is connected with described gaseous phase outlet, and described stabilizer is provided with light hydrocarbon outlet and stable gasoline outlet, and the outlet of described stable gasoline is connected setting with essence phenol device respectively with the outlet of described top recycle oil；
Hydrogenation plant, is arranged with described gas-oil outlet.
Described fractionating column is additionally provided with tail oil outlet, and the outlet of described tail oil is connected with described raw oil import.
Also including the surge tank and the preheating furnace that are sequentially connected with, the outlet of described preheating furnace is connected with described raw oil import.
Also including the knockout drum and the heater that are sequentially connected with, the import of described knockout drum is connected with described gaseous phase outlet, and the outlet of described heater is connected setting with the import of described stabilizer；
Described knockout drum is provided with rich gas outlet, sour water outlet and raw gasoline outlet, and the outlet of described raw gasoline is connected with the import of described heater.
Also including return tank, its import is connected with the outlet of described light hydrocarbon, and the outlet of described return tank is arranged with first inlet communication on described stabilizer and diesel oil absorption tower respectively, and the outlet on described diesel oil absorption tower is connected with the import of described hydrogenation plant；
The outlet of described gas-oil is connected setting with second import on described diesel oil absorption tower and the import of described hydrogenation plant respectively.
It is additionally provided with heating furnace between the outlet of described flash oil and the import of described coke drum；
Arranging guide float valve tray on the top of described fractionating column, arranging in the bottom of described fractionating column with horizontal direction is 15-35 ° of tilted-putted herringbone baffle plate, arranges slurry oil stirring line in the bottom of described fractionating column.
The technique scheme of the present invention has the advantage that
1, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil provided by the invention, raw gasoline is carried out separating treatment initiatively to remove the light hydrocarbon in raw gasoline, obtain stable gasoline, and stable gasoline is merged as carbolic oil with the top recycle oil fractionated out.Compared with directly raw gasoline being used for Petroleum processed with existing coal tar crude phenols technology, the method of the present invention using appropriately processed for the raw gasoline accounting for carbolic oil total amount 40wt% in coal tar as carbolic oil, drastically increase the yield of carbolic oil so that utilize the yield of coal tar carbolic oil to maximize.
2, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention, also the light hydrocarbon of elimination from raw gasoline is mixed the raw material as hydrogenation plant with the gas-oil component fractionated out, the present invention is made to utilize the maximized maximization simultaneously also achieving diesel yield of yield of coal tar carbolic oil on the one hand, the comprehensive utilization ratio of coal tar is greatly improved, make on the other hand compared with raw gasoline is directly used for Petroleum processed with existing coal tar crude phenols technology by the method for the present invention, by the phenolic component in raw gasoline is separated, optionally only the light hydrocarbon in raw gasoline is used for Petroleum processed, thus can reduce the difficulty that follow-up hydrogenation processes, it is also beneficial to improve the quality of refined diesel oil and Petroleum.
3, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention, by flash oil being carried out delayed coking when recycle ratio is 0.3-0.8, the technique of the present invention is made to increase the single pass cracking degree of depth to flash oil on the one hand, advantageously reduce the tenor in pitch coke and sulfur content, also reduce the sulfur in diesel oil and naphtha product, nitrogen content equally, thus ensureing that the product obtained by the present invention has significantly high quality；Make the coke powder contained by coal tar raw material, coal dust etc. can almost be completely converted into pitch coke in coke drum on the other hand to deposit, effectively prevent the raw oil coking at Fractionator Bottom and furnace tubing, be conducive to whole technique longtime running continuously and stably, also widened the raw material scope of application of the method for the invention so that the method for the present invention can be suitably used for from all different types of coal tar particularly containing producing carbolic oil and diesel oil fine coal tar simultaneously.
Additionally, owing to the metal complex in coal tar with porphyrin structure being shown significantly high affinity containing the surface of the dust such as coke powder contained in fine coal tar, coal dust, the organo-metallic compound in coal tar is made to can be adsorbed on solid coal, burnt surface, reduce the severity of green coke, therefore, the present invention utilizes this characteristic containing fine coal tar can improve product liquid and receives so that the yield of the present invention fluid product to prepare for raw material containing fine coal tar improves 1-2% compared with the yield adopted without the fluid product obtained by the coal tar of dust.
4, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention, by coal tar is carried out flash distillation process, the flashed vapour obtained just can be directly used for fractional distillation without processing through coking, is conducive to improving the treating capacity of whole technique, also can reduce the energy consumption of device simultaneously.
5, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention, by adopting preheating furnace to be preheated to after 260-320 DEG C by coal tar and mix with the tail oil fractionated out again, to avoid adopting conventional heat exchanger easy condensation component in coal tar in heat transfer process to cause that heat exchanger blocks because of coking, thus it is advantageously ensured that the continuous-stable longtime running of whole technique.
6, the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention, by obtaining sweet gas after the rich gas fractionated out desulfurization, being used for sweet gas again adding hot coal tar and flash oil, thus having saved the energy, advantageously reducing the energy consumption of whole process unit.
Additionally; the sour water fractionated out has been carried out processing obtaining liquefied ammonia and sulfur by the of the present invention method utilizing coal tar maximization to prepare carbolic oil and diesel oil further; not only reduce pollutant emission; be conducive to environmental conservation; also make the method for the present invention while utilizing coal tar maximization to prepare carbolic oil and diesel oil can the industrial chemicals such as by-product liquefied ammonia, sulfur, also improve the economic benefit of the method for the invention undoubtedly.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme in the specific embodiment of the invention, below the accompanying drawing used required during detailed description of the invention is described is briefly described, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the flow chart of the method utilizing coal tar maximization to prepare carbolic oil and diesel oil of the present invention.
Wherein, accompanying drawing labelling is as follows:
1-surge tank；2-raw oil pump；3-preheating furnace；4-flash column；5-furnace charge pump；6-heating furnace；7-cross valve；8-coke drum；9-fractionating column；10-column bottoms pump；11-the first water cooler；12-knockout drum；13-raw gasoline pump；14-heater；15-stabilizer；16-stable gasoline pump；17-reboiler；18-the second water cooler；19-return tank；20-reflux pump；21-diesel oil absorption tower；22-absorbs column bottoms pump.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is clearly and completely described, it is clear that described embodiment is a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
In describing the invention, unless otherwise clearly defined and limited, term " being connected ", " connection " should be interpreted broadly, for instance, it is possible to it is fixing connection, it is also possible to be removably connect, or connect integratedly；Can be mechanically connected, it is also possible to be electrical connection；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, it is possible to be the connection of two element internals.For the ordinary skill in the art, it is possible to concrete condition understands above-mentioned term concrete meaning in the present invention.Term " first ", " second " only for descriptive purposes, and it is not intended that instruction or hint relative importance.
As long as just can be combined with each other additionally, technical characteristic involved in invention described below difference embodiment does not constitute conflict each other.
Hydrotreating step in the method for the invention is ordinary skill in the art means, and the process conditions of hydrotreatment can carry out Reasonable adjustment according to actual condition.In the following embodiments, the inlet pressure of hydrogenation reactor is not more than 15MPa (hydrogen dividing potential drop), and initial reaction temperature is 300-390 DEG C (beds mean temperature), and volume space velocity is 0.4-4.0h-1, hydrogen-oil ratio is 500-3000Nm3/m3。
Embodiment 1
Utilize, described in the present embodiment, the method that coal tar maximization prepares carbolic oil and diesel oil, including:
(1) medium temperature coal tar is sent in flash column 4,0.22MPa, 290 DEG C when coal tar is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
(2) described flash oil enters in coke drum 8, carries out delayed coking when 480 DEG C, 0.2MPa and recycle ratio are 0.3, occurs cracking and condensation reaction to generate oil gas and pitch coke, and pitch coke discharges coke drum by hydraulic decoking；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.16MPa, tower top temperature carry out fractional distillation process when being 130 DEG C, and fractionating column respectively is isolated by raw gasoline, top recycle oil, gas-oil and tail oil from top to bottom；
(4) heating of described raw gasoline is easily separated process to remove light hydrocarbon therein to sending into after 110 DEG C in stabilizer 15, obtains stable gasoline, more described stable gasoline is merged with described top recycle oil deliver to smart phenol device as carbolic oil raw material；
(5) described gas-oil enters hydrogenation plant to carry out hydrotreatment, obtains refined diesel oil and Petroleum.
Embodiment 2
Utilize, described in the present embodiment, the method that coal tar maximization prepares carbolic oil and diesel oil, including:
(1) tar containing fine coal is delivered in preheating furnace 3 and is preheated to after 300 DEG C and forms miscella with the part tail oil mixed heat transfer from fractionating column 9, miscella is sent into flash column 4 again, 0.11MPa, 320 DEG C when miscella is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
Wherein said is 10wt% containing the dust content in fine coal tar, and described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
(2) the heated stove 6 of described flash oil enters in coke drum 8 after being warming up to 480 DEG C, delayed coking is carried out when 480 DEG C, 0.1MPa and recycle ratio are 0.55, occurring cracking and condensation reaction to generate oil gas and pitch coke, pitch coke discharges coke drum by hydraulic decoking；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.06MPa, tower top temperature carry out fractional distillation process when being 115 DEG C, and fractionating column respectively is isolated by gas phase, top recycle oil, gas-oil and tail oil from top to bottom；
Wherein said gas phase enters knockout drum 12 and carries out three phase separation, respectively obtains raw gasoline, rich gas and sour water；
(4) heating of described raw gasoline is easily separated process to remove light hydrocarbon therein to sending into after 130 DEG C in stabilizer 15, obtains stable gasoline, more described stable gasoline is merged with described top recycle oil deliver to smart phenol device as carbolic oil raw material；
(5) described gas-oil enters hydrogenation plant to carry out hydrotreatment, obtains refined diesel oil and Petroleum.
Embodiment 3
Utilize, described in the present embodiment, the method that coal tar maximization prepares carbolic oil and diesel oil, including:
(1) buffered for the tar containing fine coal tank 1 is delivered in preheating furnace 3 and is preheated to after 320 DEG C and forms miscella with the part tail oil mixed heat transfer from fractionating column 9, miscella is sent into flash column 4 again, 0.32MPa, 335 DEG C when miscella is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
Wherein said is 5.5wt% containing the dust content in fine coal tar, and described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
(2) the heated stove 6 of described flash oil enters in coke drum 8 after being warming up to 420 DEG C, delayed coking is carried out when 420 DEG C, 0.3MPa and recycle ratio are 0.8, occurring cracking and condensation reaction to generate oil gas and pitch coke, pitch coke discharges coke drum by hydraulic decoking；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.25MPa, tower top temperature carry out fractional distillation process when being 130 DEG C, and fractionating column respectively is isolated by gas phase, top recycle oil, gas-oil and tail oil from top to bottom；
Wherein said gas phase enters knockout drum 12 after the first water cooler 11 heat exchange cooling and carries out three phase separation, respectively obtains raw gasoline, rich gas and sour water；
(4) heating of described raw gasoline is easily separated process to remove light hydrocarbon therein to sending into after 115 DEG C in stabilizer 15, obtains stable gasoline, more described stable gasoline is merged with described top recycle oil deliver to smart phenol device as carbolic oil raw material；
(5) the cooled post liquefaction part of described light hydrocarbon returns the tower top of stabilizer 15 to control tower top temperature, and remainder enters hydrogenation plant to carry out hydrotreatment after mixing with described gas-oil, obtains refined diesel oil and Petroleum.
Embodiment 4
Utilize, described in the present embodiment, the method that coal tar maximization prepares carbolic oil and diesel oil, including:
(1) buffered for the tar containing fine coal tank 1 is delivered in preheating furnace 3 and is preheated to after 260 DEG C and forms miscella with the part tail oil mixed heat transfer from fractionating column 9, miscella is sent into flash column 4 again, 0.22MPa, 280 DEG C when miscella is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
Wherein said is 1wt% containing the dust content in fine coal tar, and described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
(2) the heated stove 6 of described flash oil enters in coke drum 8 after being warming up to 490 DEG C, delayed coking is carried out when 490 DEG C, 0.2MPa and recycle ratio are 0.4, occurring cracking and condensation reaction to generate oil gas and pitch coke, pitch coke discharges coke drum by waterpower coke discharging；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.16MPa, tower top temperature carry out fractional distillation process when being 125 DEG C, and fractionating column 9 respectively is isolated by gas phase, top recycle oil, gas-oil and tail oil from top to bottom；
Wherein, described gas phase enters knockout drum 12 after the first water cooler 11 heat exchange cooling and carries out three phase separation, respectively obtains raw gasoline, rich gas and sour water；The sweet gas that described rich gas obtains after desulfurization is for heating described coal tar and/or described flash oil, described sour water is carried out stripping process, obtaining thick ammonia and sour gas, described thick ammonia obtains liquefied ammonia after ammonia refining, and described sour gas obtains sulfur after Cross unit processes；
(4) heating of described raw gasoline is easily separated process to remove light hydrocarbon therein to sending into after 100 DEG C in stabilizer 15, obtains stable gasoline, more described stable gasoline is merged with described top recycle oil deliver to smart phenol device as carbolic oil raw material；
(5) described light hydrocarbon enters in return tank 19 after the second water cooler 18 is cooled to 40 DEG C and is easily separated buffering, liquid phase component in return tank 19 is after reflux pump 20 boosts, part returns the tower top of stabilizer 15 to control tower top temperature, another part enters the bottom on diesel oil absorption tower 21, a part of washing and recycling in the gas-oil obtained by step (3), the gas-oil absorbing light hydrocarbon is mixed and fed into hydrogenation plant to carry out hydrotreatment with remainder gas-oil after absorbing column bottoms pump 22 boosting, obtains refined diesel oil and Petroleum.
Embodiment 5
Utilize, described in the present embodiment, the method that coal tar maximization prepares carbolic oil and diesel oil, including:
(1) send in preheating furnace 3 by raw oil pump 2 after buffered tank 1 balance of the tar containing fine coal, it is preheated to after 290 DEG C until coal tar and forms miscella with the part tail oil mixed heat transfer after column bottoms pump 10 boosts from fractionating column 9, miscella is sent into flash column 4 again, 0.15MPa, 305 DEG C when miscella is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
Wherein said is 3wt% containing the dust content in fine coal tar, and described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
(2) the heated stove feed pump 5 of described flash oil is delivered in heating furnace 6, enter in coke drum 8 again through cross valve 7 after being warming up to 455 DEG C, delayed coking is carried out when 455 DEG C, 0.1MPa and recycle ratio are 0.6, occurring cracking and condensation reaction to generate oil gas and pitch coke, pitch coke discharges coke drum by hydraulic decoking；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.06MPa, tower top temperature carry out fractional distillation process when being 115 DEG C, and fractionating column respectively is isolated by gas phase, top recycle oil, gas-oil and tail oil from top to bottom；
Wherein, described gas phase enters knockout drum 12 after the first water cooler 11 heat exchange cooling and carries out three phase separation, respectively obtains raw gasoline, rich gas and sour water；The sweet gas that described rich gas obtains after desulfurization is for heating described coal tar and/or described flash oil, described sour water is carried out stripping process, obtaining thick ammonia and sour gas, described thick ammonia obtains liquefied ammonia after ammonia refining, and described sour gas obtains sulfur after Cross unit processes；
(4) described raw gasoline is sent in heater 14 through raw gasoline pump 13, to be heated it is easily separated process to remove light hydrocarbon therein to entering back into stabilizer 15 after 100 DEG C, obtaining stable gasoline, described stable gasoline merges with described top recycle oil after stable gasoline pump 16 boosts delivers to essence phenol device as carbolic oil raw material；
(5) described light hydrocarbon enters in return tank 19 after the second water cooler 18 is cooled to 40 DEG C and is easily separated buffering, liquid phase component in return tank is after reflux pump 20 boosts, part returns the tower top of stabilizer 15 to control tower top temperature, another part enters the bottom on diesel oil absorption tower 21, a part of washing and recycling in the gas-oil obtained by step (3), the gas-oil absorbing light hydrocarbon is mixed and fed into hydrogenation plant to carry out hydrotreatment with remainder gas-oil after absorbing column bottoms pump 22 boosting, obtains refined diesel oil and Petroleum.
Embodiment 6
Method described in embodiment of the present invention 1-5 is to be realized by the following device utilizing coal tar maximization to prepare carbolic oil and diesel oil:
The device of carbolic oil and diesel oil is prepared in the coal tar maximization that utilizes described in the present embodiment, as it is shown in figure 1, include:
Flash column 4, is provided with raw oil import, flashed vapour outlet and flash oil outlet；
Coke drum 8, its import is connected setting with the outlet of described flash oil, and described coke drum 8 is provided with pitch coke outlet and oil gas vent；
Connecting, with the outlet of described flashed vapour and described oil gas vent, the fractionating column 9 arranged respectively, described fractionating column 9 is provided with gaseous phase outlet, top recycle oil outlet and gas-oil outlet；
Stabilizer 15, its import is connected with described gaseous phase outlet, and described stabilizer 15 is provided with light hydrocarbon outlet and stable gasoline outlet, and the outlet of described stable gasoline is connected setting with essence phenol device respectively with the outlet of described top recycle oil；
Hydrogenation plant, is arranged with described gas-oil outlet.
As preferred embodiment, the present embodiment is additionally provided with heating furnace 6 between the outlet of described flash oil and the import of described coke drum 8, and described coke drum 8 is two coke drums in parallel, and when one in said two coke drum is for green coke, another is used for devoking.
As selectable embodiment, fractionating column 9 described in the present embodiment is additionally provided with tail oil outlet, and the outlet of described tail oil is connected with described raw oil import.Additionally, the device described in the present embodiment also includes the surge tank 1 and the preheating furnace 3 that are sequentially connected with setting, the outlet of described preheating furnace 3 is connected with described raw oil import.
Embodiment as changeable type, device described in the present embodiment farther includes the knockout drum 12 and the heater 14 that are sequentially connected with, the import of described knockout drum 12 is connected with described gaseous phase outlet, and the outlet of described heater 14 is connected setting with the import of described stabilizer 15；Described knockout drum 12 is provided with rich gas outlet, sour water outlet and raw gasoline outlet, and the outlet of described raw gasoline is connected with the import of described heater 14.
Still more preferably, device described in the present embodiment also includes return tank 19, its import is connected with the outlet of described light hydrocarbon, the outlet of described return tank 19 is arranged with first inlet communication on described stabilizer 15 and diesel oil absorption tower 21 respectively, and the outlet on described diesel oil absorption tower 21 is connected with the import of described hydrogenation plant.In the present embodiment, the outlet of described gas-oil is connected setting with second import on described diesel oil absorption tower 21 and the import of described hydrogenation plant respectively.
As interchangeable embodiment, the present embodiment arranges guide float valve tray on the top of described fractionating column 9, arranging in the bottom of described fractionating column 9 with horizontal direction is 15-35 ° of tilted-putted herringbone baffle plate, arranges slurry oil stirring line in the bottom of described fractionating column 9 to prevent liquid in tower bottom sediments coking.
Comparative example
Utilize, described in this comparative example, the method that coal tar prepares carbolic oil and diesel oil, including:
(1) send in preheating furnace 3 by raw oil pump 2 after buffered tank 1 balance of the tar containing fine coal, it is preheated to after 290 DEG C until coal tar and forms miscella with the part tail oil mixed heat transfer after column bottoms pump 10 boosts from fractionating column 9, miscella is sent into flash column 4 again, 0.15MPa, 305 DEG C when miscella is carried out flash distillation process, in overhead collection flashed vapour, in tower, liquid is flash oil；
Wherein said is 3wt% containing the dust content in fine coal tar, and described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
(2) the heated stove feed pump 5 of described flash oil is delivered in heating furnace 6, enter in coke drum 8 again through cross valve 7 after being warming up to 455 DEG C, delayed coking is carried out when 455 DEG C, 0.1MPa and recycle ratio are 0.6, occurring cracking and condensation reaction to generate oil gas and pitch coke, pitch coke discharges coke drum by hydraulic decoking；
(3) flashed vapour of step (1) and the oil gas of step (2) all enter in fractionating column 9 at tower top pressure is that 0.06MPa, tower top temperature carry out fractional distillation process when being 115 DEG C, and fractionating column respectively is isolated by gas phase, top recycle oil, gas-oil and tail oil from top to bottom；
Wherein, described top recycle oil is carbolic oil raw material；Described gas phase enters knockout drum 12 after the first water cooler 11 heat exchange cooling and carries out three phase separation, respectively obtains raw gasoline, rich gas and sour water；Described raw gasoline and described gas-oil enter in hydrogenation plant jointly to carry out hydrotreatment, obtain refined diesel oil and Petroleum.
The Nature comparison of table 1 embodiment 5 and comparative example products obtained therefrom
As can be seen from Table 1, compared with comparative example, the yield of the carbolic oil that embodiment 5 prepares substantially increases, and nitrogen, sulfur content in the refined diesel oil obtained and Petroleum are all relatively low, illustrate that method of the present invention by being separated into light hydrocarbon and two components of stable gasoline by raw gasoline, light hydrocarbon is used as the raw material of Hydrogenation Petroleum again, and using stable gasoline as carbolic oil so that the present invention utilizes cleaning of the maximized maximization that simultaneously also ensure that diesel yield of yield of coal tar carbolic oil and diesel oil and Petroleum quality.
Obviously, above-described embodiment is only for clearly demonstrating example, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the apparent change thus extended out or variation are still among the protection domain of the invention.
Claims (14)
1. utilize the method that carbolic oil and diesel oil are prepared in coal tar maximization, including:
(1) coal tar is carried out flash distillation process, collect the flashed vapour and flash oil that obtain respectively；
(2) described flash oil is carried out delayed coking, obtain oil gas and pitch coke；
(3) described oil gas and described flashed vapour are carried out fractional distillation process jointly, obtain raw gasoline, top recycle oil, gas-oil and tail oil；
(4) described raw gasoline is easily separated process and obtains stable gasoline removing light hydrocarbon, described stable gasoline is merged as carbolic oil with described top recycle oil；
(5) described gas-oil is carried out hydrotreatment, obtain refined diesel oil and Petroleum.
2. the method utilizing coal tar maximization to prepare carbolic oil and diesel oil according to claim 1, it is characterised in that described coal tar be containing 1-10wt% dust containing fine coal tar, described dust is coke powder and/or coal dust, and the particle diameter of described dust is less than 100 μm.
3. the method utilizing coal tar maximization to prepare carbolic oil and diesel oil according to claim 1 and 2, it is characterized in that, in step (1), after described coal tar is preheated to 260-320 DEG C, it is mixed to form miscella with the described tail oil of part, described miscella is carried out described flash distillation process.
4. utilize, according to any one of claim 1-3, the method that coal tar maximization prepares carbolic oil and diesel oil, it is characterized in that, in step (2), described delayed coking is to carry out when 420-490 DEG C, 0.1-0.3MPa and recycle ratio are 0.3-0.8.
5. utilize, according to any one of claim 1-4, the method that coal tar maximization prepares carbolic oil and diesel oil, it is characterized in that, in step (3), carry out three phase separation after described fractional distillation is processed the gas phase cooling obtained, respectively obtain rich gas, sour water and described raw gasoline.
6. the method utilizing coal tar maximization to prepare carbolic oil and diesel oil according to claim 5, it is characterised in that the sweet gas that described rich gas obtains after desulfurization is for heating described coal tar and/or described flash oil.
7. utilize, according to claim 5 or 6, the method that coal tar maximization prepares carbolic oil and diesel oil, it is characterised in that described sour water is carried out stripping process, obtains thick ammonia and sour gas；Described thick ammonia obtains liquefied ammonia after ammonia refining, and described sour gas obtains sulfur after Cross unit processes.
8. utilizing, according to any one of claim 1-7, the method that coal tar maximization prepares carbolic oil and diesel oil, it is characterised in that in step (4), the heating of described raw gasoline is easily separated process to entering in stabilizer after 100-130 DEG C；Described light hydrocarbon cooled post liquefaction part returns in described stabilizer as overhead reflux, and another part mixes with described gas-oil and carries out described hydrotreatment.
9. utilize coal tar maximization to prepare a device for carbolic oil and diesel oil, including:
Flash column (4), is provided with raw oil import, flashed vapour outlet and flash oil outlet；
Coke drum (8), its import is connected setting with the outlet of described flash oil, and described coke drum (8) is provided with pitch coke outlet and oil gas vent；
Connecting, with the outlet of described flashed vapour and described oil gas vent, the fractionating column (9) arranged respectively, described fractionating column (9) is provided with gaseous phase outlet, top recycle oil outlet and gas-oil outlet；
Stabilizer (15), its import is connected with described gaseous phase outlet, and described stabilizer (15) is provided with light hydrocarbon outlet and stable gasoline outlet, and the outlet of described stable gasoline is connected setting with essence phenol device respectively with the outlet of described top recycle oil；
Hydrogenation plant, is arranged with described gas-oil outlet.
10. the device utilizing coal tar maximization to prepare carbolic oil and diesel oil according to claim 9, it is characterised in that described fractionating column (9) is additionally provided with tail oil outlet, and the outlet of described tail oil is connected with described raw oil import.
11. the device utilizing coal tar maximization to prepare carbolic oil and diesel oil according to claim 10, it is characterized in that, also including the surge tank (1) and the preheating furnace (3) that are sequentially connected with, the outlet of described preheating furnace (3) is connected with described raw oil import.
12. the device of carbolic oil and diesel oil is prepared in the coal tar maximization that utilizes according to any one of claim 9-11, it is characterized in that, also include the knockout drum (12) and the heater (14) that are sequentially connected with, the import of described knockout drum (12) is connected with described gaseous phase outlet, and the outlet of described heater (14) is connected setting with the import of described stabilizer (15)；
Described knockout drum (12) is provided with rich gas outlet, sour water outlet and raw gasoline outlet, and the outlet of described raw gasoline is connected with the import of described heater (14).
13. the device of carbolic oil and diesel oil is prepared in the coal tar maximization that utilizes according to any one of claim 9-12, it is characterized in that, also include return tank (19), its import is connected with the outlet of described light hydrocarbon, the outlet of described return tank (19) is arranged with the first inlet communication of described stabilizer (15) and diesel oil absorption tower (21) respectively, and the outlet of described diesel oil absorption tower (21) is connected with the import of described hydrogenation plant；
The outlet of described gas-oil is connected setting with described second import of diesel oil absorption tower (21) and the import of described hydrogenation plant respectively.
14. the device of carbolic oil and diesel oil is prepared in the coal tar maximization that utilizes according to any one of claim 9-13, it is characterised in that be additionally provided with heating furnace (6) between the outlet of described flash oil and the import of described coke drum (8)；
On the top of described fractionating column (9), guide float valve tray is set, arranging in the bottom of described fractionating column (9) with horizontal direction is 15-35 ° of tilted-putted herringbone baffle plate, arranges slurry oil stirring line in the bottom of described fractionating column (9).
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