CN109181770A

CN109181770A - A method of refining production oil product and chemicals altogether for inferior heavy oil, coal

Info

Publication number: CN109181770A
Application number: CN201810755434.0A
Authority: CN
Inventors: 王小英
Original assignee: Shanghai Yingbao Energy Chemical Technology Co Ltd
Current assignee: Shanghai Jun Ming Chemical Engineering Design Co. Ltd.
Priority date: 2018-07-11
Filing date: 2018-07-11
Publication date: 2019-01-11
Anticipated expiration: 2038-07-11
Also published as: CN109181770B

Abstract

The method that the present invention provides a kind of to refine production oil product and chemicals for inferior heavy oil, coal altogether, coal dust, hydrogen supply dissolvent oil and catalyst are mixed with coal, it refines in reactor and cracks altogether in kerosene, hot high score oil O1 isolated to pyrolysis product, vacuum fractionation is carried out to hot high score oil O1 to obtain to contain solid Residual oil containing solid Residual oil and being separated by solid-liquid separation to obtain Residual oil；Inferior heavy oil is blended in fluidized bed reactor with Residual oil and is hydrocracked, hot high score oil O2 isolated to crackate, vacuum fractionation is carried out to hot high score oil O2 and is recycled into the preparation of coal using decompressed wax oil as hydrogen supply dissolvent oil in fractionating column side take-off decompressed wax oil；A kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention, coal conversion ratio and oil product yield are improved, the coking problem of system is alleviated, has delayed catalyst inactivation, it is conducive to extend the operation cycle of production equipment, reduces production cost.

Description

A method of refining production oil product and chemicals altogether for inferior heavy oil, coal

Technical field

The method that the present invention relates to a kind of to refine production oil product and chemicals for inferior heavy oil, coal altogether, belongs to petrochemical industry And technical field of coal chemical industry, more belong to clean coal and utilizes technical field.

Background technique

DCL/Direct coal liquefaction and coal, oil refine two key areas that technology is semicoke technology altogether.Direct coal liquefaction process be by Fine coal is mixed with circulation solvent, reacts under certain temperature, pressure condition with hydrogen, the organic matter of coal is made to be converted into liquid Carburetion；Again by desulfurization, denitrogenation, further improves liquefaction oil quality, product is enable to produce fortune in general oil plant Defeated fuel and chemical products.The advantages of DCL/Direct coal liquefaction is oil yield height, and the thermal efficiency is high；Major defect is the operation of hydrogenation technique Condition is harsher.And refining technology is that a kind of coal to grow up on the basis of direct coal liquefaction technology and heavy oil are total to altogether for coal, oil With the technology of processing, which has the characteristics that be completed at the same time two processes of heavy oil modification and coal liquefaction, be effective use coal with The important means of inferior heavy oil.

Compared with direct coal liquefaction technology, refining technology has the advantage that and can make full use of having for reactor altogether for coal, oil Volume is imitated, the processing capacity of process units and the production efficiency of the technical process are improved；Cooperateing between coal and heavy oil simultaneously Effect, so that the oil products such as generation oil gasoline, diesel oil easier to process for becoming qualification that kerosene refines altogether；Protium in residual oil compares coal Protium content it is high, during coal, oil refining altogether, hydrogen consumption is reduced, and hydrogen utilization rate increases substantially, can effectively reduce energy consumption and Equipment investment；Minor metallic element (such as iron, nickel) in heavy oil can be used as hydrogenation active component, promote hydrogenation reaction into Row, effectively raises the quality of oil product.

Refining is broken at the weak cross-bond of coal under conditions of high temperature, high pressure altogether for coal, oil, forms size not Deng coal free radical fragment, coal free radical fragment receives hydrogen in hydrogen supply dissolvent and hydrogen atmosphere, or coal intramolecular hydrogen occurs and resets Transfer, and hydrogenolysis, cracking and the self-stabilizationization reaction of series of parallel sequence are carried out, generate the lower product of molecular weight.Coal, During oily refining altogether, coal and heavy oil not fully respective independent reaction, and have very strong reciprocation.Heavy oil is both reactant, While carrying out hydrocracking reaction, and the solvent as coal liquefaction, affect the conversion process of coal.If heavy oil tool used There is good hydrogen supply capacity, coal and heavy oil have good synergistic effect, and refining oil tech is better than often to a certain extent altogether for coal, oil Advise direct coal liquefaction technology；But if heavy oil used does not have good hydrogen supply capacity, oil yield cannot be not only improved, can also Oil yield is reduced, the generation of coking phenomenon is even resulted in, causes reactor plugs, aggravate the inactivation of catalyst, thus shadow The device production cycle in actual production process is rung, the reduction of production energy consumption and production cost is unfavorable for.

Therefore, in coal, oil altogether refining technology, how heavy oil is effectively handled, produces out suitable oil ingredient and makees It is one of the emphasis that kerosene refines new technology development altogether for hydrogen supply dissolvent.In the prior art, heavy is mainly reduced by thermal cracking Condensed-nuclei aromatics in mink cell focus, is hydrogenated into the hydrogen supply dissolvent of fractional saturation by the viscosity of oil.

The method of coal tar disclosed in CN104178197A and coal coreaction liquid fuel was prepared, includes the following steps: (1) Coal dust, coal tar, hydrogenation catalyst are mixed to get coal；(2) after above-mentioned coal being preheated to 350~410 DEG C, successively Carrying out level-one adds hydrogen and secondary hydrogenation to react；(3) product after secondary hydrogenation reacts carries out level-one gas-liquid separation, obtains gas phase Substance and liquid phase substance, the gaseous substance obtain hydrogen and light oil through second level gas-liquid separation again；At least part liquid Phase substance obtains heavy oil and liquefied residue through vacuum distillation；(4) by the step (3) the heavy oil and the light oil it is mixed Hydrogenated reaction again, is prepared liquid fuel after conjunction.This method is using the portion generated after coal tar and floating bed hydrogenation reaction The hydrogen supply dissolvent for dividing mink cell focus to refine reaction altogether as kerosene.Middle coalite tar raw material is inherently with short-side chain condensed-nuclei aromatics Main hydrocarbon structure composition, after a thermal cracking, saturated hydrocarbons side chain is broken substantially, and generating oil is shorter and less side chain The generation oil of this spline structure is recycled back to suspended-bed reactor by condensed-nuclei aromatics mixture, and part oil is also recycled back to outstanding more than once Floating bed reactor is reacted, and only meeting greater proportion occurs condensation reaction generation coking or maintains molecular structure constant, to drop Low oil product yield, the generation of coking be easy to cause kerosene to refine the blocking of reactor altogether.

A kind of coal tar disclosed in CN106433775A is total to smelting method and its device, wherein smelting method includes by heavy altogether Oil does not add hydrogen circulation solvent and the mixing of the first catalyst, slurry oil is made, obtained slurry oil is in slurry bed system or bubbling bed reactor Middle progress hydrocracking reaction, reaction product separation, obtains the first light fraction oil and the first heavy distillate；By the first heavy Distillate, coal dust, the mixing of the second catalyst, are made coal, second of hydrocracking reaction are carried out in paste state bed reactor, Reaction product is separated, the second light fraction oil, the second heavy distillate and residue are obtained；Second heavy distillate conduct Not plus hydrogen recycles solvent, the preparation for slurry oil；By the first light fraction oil and the second light fraction oil in fixed bed reactors Middle progress third adds hydrogen upgrading, and reaction product separation obtains liquid fuel.The method will be hydrocracked instead by paste state bed reactor Ying Houwei adds the mink cell focus of hydrogen subsequent and feeding slurry bed system or bubbling bed reactor are hydrocracked, and the purpose is to mink cell focus In macromolecular pitch it is as much as possible be cracked into small molecule clean or white, but the ratio that occurs of this cracking reaction compared with Small, thermal cracking temperature is higher, and mink cell focus is easy to appear coking phenomenon, reduces overall oil yield.

CN104087339A discloses a kind of method that miscellaneous oily, coal and coal tar hydrogenating refine altogether, and this method is first to coal tar Raw material carries out distillation processing, is divided into≤320 DEG C of light fraction and 320 DEG C of > of heavy distillate；The heavy end that will be obtained Oil enters paste state bed reactor after being mixed and made into coal with coal, miscellaneous oil and catalyst, in 400~455 DEG C of reaction temperature, reaction 8~19MPa of pressure and hydrogen to oil volume ratio react under conditions of being 800~1200, and reaction product is separated, and isolated subtracts Pressure oil and≤320 DEG C of light fractions enter fixed bed and carry out hydrofinishing, and final fractionation obtains gasoline, diesel oil and 350~500 DEG C Mink cell focus；The mink cell focus is recirculated back to coal preparation unit as circulation hydrogen supply dissolvent.Following process light oil and decompression Oil plus hydrogen restructuring unit use fixed bed hydrogenation technique known in the art, when in raw material contain high metal, high asphalitine Or when high colloid, device can have that fast catalyst inactivation, easy coking, bed layer pressure lifting is fast, the device cycle of operation is short, raw material is suitable Answer the drawbacks such as narrow range.

CN107987861A discloses the combined method of a kind of high aromatic oil hydrogenation process and direct hydrogenation liquefaction of coal process, High aromatic oil such as coal tar AF is fractionated and is turned for distilled oil AFD and residual oil AFV, the hydrogenated refining reaction process AHR of distilled oil AFD It turns to material flow A SH, material flow A SH and coal dust ACF the preparation coal rich in hydrogen supply the hydrocarbon component and enters direct hydrogenation liquefaction of coal process BHR, AFV can enter HBR joint processing；Direct hydrogenation liquefaction of coal process gained circulation preferably with coal dust BCF, coal dust BCF supplies Hydrogen solvent BFKSH joint operation.The component for using fractionation to handle high aromatic oil in this method, especially residue fraction, Enter direct hydrogenation liquefaction of coal process as circulation hydrogen supply dissolvent, and be recycled in systems, this not only bad for Ensure that the hydrogen supply capacity for recycling hydrogen supply dissolvent aggravates the inactivation of catalyst it also occur that condensation reaction causes coking, is unfavorable for mentioning High oil product yield, or even cause reactor plugs.

Summary of the invention

In view of this, the present invention is directed to propose it is a kind of for inferior heavy oil, coal altogether refine production oil product and chemicals method, To solve the problems, such as existing kerosene, oil product yield present in refining technology is lower altogether and the easy coking of device.

In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:

A method of production oil product and chemicals are refined altogether for inferior heavy oil, coal, by coal dust, hydrogen supply dissolvent oil and catalysis Agent is mixed with coal, refines in reactor and cracks altogether in kerosene, hot high score oil O1 isolated to pyrolysis product, to hot high score Oily O1 carries out vacuum fractionation and obtains to contain solid Residual oil containing solid Residual oil and being separated by solid-liquid separation to obtain Residual oil；By inferior heavy oil and Residual oil It is blended in fluidized bed reactor and is hydrocracked, hot high score oil O2 isolated to crackate subtracts hot high score oil O2 Pressure fractionating is recycled into the preparation of coal using decompressed wax oil as hydrogen supply dissolvent oil in fractionating column side take-off decompressed wax oil.

Further, the coal dust includes at least one of mud coal, bituminous coal, lignite；

The inferior heavy oil includes consistency crude oil, reduced crude, decompression residuum, catalytic cracked oil pulp, deasphalted oil, visbreaking weight At least one of oil, coking heavy oil, shale oil, oil sands bitumen oil；

Wherein, solid content >=10g/L of the inferior heavy oil, Con. carbon are 10wt%~25wt%, toluene insoluble Object content is 1wt%~5wt%.

Further, a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal, including it is following Step:

S1, coal dust, hydrogen supply dissolvent oil and catalyst are mixed and made into coal；

After S2, coal mix preheating with hydrogen, refines reactor altogether into kerosene and carry out facing hydrogen heat scission reaction；

S3, kerosene refine the reaction product in reactor altogether, separate through high pressure hot separator, obtain hot high score gas G1 and Re Gao Divide oil O1；

Hot high score oil O1 in S4, step S3 enters decompression distillation system and is fractionated, isolate light oil, middle matter oil, Containing solid Residual oil；

S5, Residual oil and semicoke are isolated through solid-liquid separation system containing solid Residual oil；

Residual oil in S6, inferior heavy oil and step S5 carries out together into boiling bed system plus hydrogen；

S7, fluidized bed reactor reaction product are separated through high pressure hot separator, obtain hot high score gas G2 and hot high score Oily O2；

Hot high score oil O2 in S8, step S7, which is sent to vacuum fractionation tower, to be separated, and depressurizes wax in fractionating column side take-off Oil produces boiling bed hydrogenation tail oil at fractionation column bottom；

Decompressed wax oil in S9, step S8, which is recycled back in step S1, carries out coal preparation as hydrogen supply dissolvent oil；

Hot high score gas in hot high score gas G1 in S10, step S3, the light oil in step S4, middle matter oil and step S7 G2 is sent into fixed bed hydrogenation system together, prepares oil product.

Further, in the method, the boiling bed hydrogenation tail oil in step S8 is sent to catalytic cracking alkene, aromatic hydrocarbons Device；

Semicoke in step S5 is Filter Tuber For Clean Coal, can sell, also be able to enter Hydrogen Unit, through gasification, water-gas Hydrogen is produced in transformation, gas purification, refines reactor, the boiling bed system in step S6, step altogether for the kerosene in step S2 Fixed bed hydrogenation system in S10 uses.

Further, in step s 6, inferior heavy oil enters before fluidized bed reactor, is located in advance to inferior heavy oil Reason.

Further, the pretreatment is to carry out the removing of solid residue to inferior heavy oil by centrifugal device 8, will be inferior It is greater than 40 μm of solids removal in heavy oil.

Further, the boiling bed system includes at least three concatenated ebullated beds；

First ebullated bed 91 is connect with centrifugal device 8 by discharge nozzle 7, and the top of the first ebullated bed 91 is provided under first Material valve is provided on expects pipe 911 and the first tandem tube 912, the first feeder pipe 911 and the first tandem tube 912, under first Expects pipe 911 is connect with major ingredient pipe 10, and the first tandem tube 912 is connect with the second ebullated bed 92；

The top of second ebullated bed 92 is provided with the second feeder pipe 921 and the second tandem tube 922,921 He of the second feeder pipe Material valve is provided on second tandem tube 922, the second feeder pipe 921 is connect with major ingredient pipe 10, the second tandem tube 922 and The connection of three ebullated beds 93；

The top of third ebullated bed 93 is provided with third feeder pipe 931, is provided with material valve on third feeder pipe 931, Third feeder pipe 931 is connect with major ingredient pipe 10；

Major ingredient pipe 10 is connect with the high pressure hot separator in step S7, for the material for passing through boiling bed hydrogenation to be delivered to It is separated in high pressure hot separator.

Further, step S6 includes:

S601, the Con. carbon of inferior heavy oil, toluene insolubles content are detected；

S602, inferior heavy oil is mixed with the Residual oil in step S5, mixture is pre-processed；

S603, judge whether the sum of Con. carbon and toluene insolubles content in inferior heavy oil≤14%；It is then to carry out Step S605；It is no, then carry out step S604；

S604, judge whether the sum of Con. carbon and toluene insolubles content in inferior heavy oil >=25%；It is then to carry out Step S606；It is no, then carry out step S607；

S605, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein boiling bed system is used only one Platform ebullated bed；

S606, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein boiling bed system at least uses Three ebullated beds；

S607, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein boiling bed system uses two Ebullated bed.

Further, in step sl, the catalyst is Ni-Co-Mo base water-soluble catalyst or Ni-Co-Mo base oil Soluble catalytic agent；The quality proportioning of the coal dust and hydrogen supply dissolvent oil is 1:1~1:3.

Further, in step s 2, it is suspended-bed reactor or paste state bed reactor that the kerosene refines reactor altogether；Coal The oily reaction temperature for refining reactor altogether is 380~470 DEG C, reaction pressure is 6~20MPa, 0.5~2h-1 of volume space velocity, hydrogen oil Volume ratio is 600:1~1500:1；

In step s 6, the hydrogenation conditions of the fluidized bed reactor are as follows: 8~20MPa of reaction pressure, reaction temperature 340~420 DEG C, 0.5~2.0h-1 of volume space velocity, hydrogen-oil ratio 400:1~1000:1.

Compared with the existing technology, of the present invention a kind of to refine production oil product and chemicals for inferior heavy oil, coal altogether Method has the advantage that

Each component that the present invention generates during being refined altogether the oily coal of coal, inferior heavy oil, using corresponding processing side Method carries out subsequent working process or circular treatment, and oil product and chemicals is made, is sufficiently opened coal resources, inferior heavy oil Hair and utilization；In addition, by floating bed hydrocracking, boiling bed hydrogenation cracking, fixed bed hydrogenation, catalytic cracking system in entire technique Alkene, aromatic device are organically combined, and are constituted a complete oily coal and are refined system altogether, have given full play to each device and workshop section The advantages of, and it farthest is hydrocracked ability using suspended-bed reactor, inferior heavy oil is effectively treated, and The preparation for entering coal using the decompressed wax oil of downstream fractionation tower side take-off as hydrogen supply dissolvent oil, makes full use of the fragrance of coal Synergistic effect between hydro carbons and the paraffin class of heavy oil can not only improve coal conversion ratio and oil product yield, and be conducive to alleviate The coking problem of reactor in system, delays the inactivation of catalyst, is conducive to extend the operation cycle of each device in system, reduces Production cost；In addition, the present invention pre-processes inferior heavy oil by the way that centrifugal device is arranged, can efficiently control into boiling The solid content of inferior heavy oil, slows down the coking situation of downstream reactor when rising a bed reactor, is conducive to improve coal conversion ratio and oil Product yield, the operation cycle of each device in extension system.

Detailed description of the invention

The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:

Fig. 1 is a kind of technique of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention Flow diagram；

Fig. 2 is to be centrifuged in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The structural schematic diagram of device；

Fig. 3 is to be centrifuged in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The front view of device；

Fig. 4 is to be centrifuged in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The schematic diagram of the exocentric structure of device；

Fig. 5 is to be centrifuged in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The operating status figure of device；

Fig. 6 is to be centrifuged in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The apocarpy figure of device；

Fig. 7 is to boil in a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal of the present invention The structural schematic diagram of bed system.

Description of symbols:

Shell 1, outer barrel 2, exocentric structure 3, interior bucket 31, middle bucket 32, through-hole 33, solid particle 4, arrangement of clutch 5, first axle 51, the second axis 52, feed pipe 6, discharge nozzle 7, centrifugal device 8, the first ebullated bed 91, the first feeder pipe 911, the first tandem tube 912, the second ebullated bed 92, the second feeder pipe 921, the second tandem tube 922, third ebullated bed 93, third feeder pipe 931, major ingredient Pipe 10.

Specific embodiment

With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention is further described, Obviously, described embodiment is only a part of the embodiments of the present invention, rather than whole embodiments.Based in the present invention Embodiment, those of ordinary skill in the art's every other embodiment obtained under the premise of not making the creative labor, It shall fall within the protection scope of the present invention.

The present invention refines technology for inferior heavy oil and coal altogether, propose it is a kind of refine altogether for inferior heavy oil, coal produce oil product and Coal dust, hydrogen supply dissolvent oil and catalyst are mixed with coal, refine in reactor and crack altogether in kerosene by the method for chemicals, Hot high score oil O1 isolated to pyrolysis product carries out vacuum fractionation to hot high score oil O1 and obtains that solid Residual oil will be contained containing solid Residual oil It is separated by solid-liquid separation to obtain Residual oil；Inferior heavy oil is blended in fluidized bed reactor with Residual oil and is hydrocracked, to crackate Isolated hot high score oil O2, wax will be depressurized in fractionating column side take-off decompressed wax oil by carrying out vacuum fractionation to hot high score oil O2 Oil is recycled into the preparation of coal as hydrogen supply dissolvent oil.

Since the arene content of inferior heavy oil is larger, heavy constituent is more, and this method farthest utilizes suspension bed to react Device is hydrocracked ability, handles inferior heavy oil, and using the pressurization wax oil of downstream fractionation tower side take-off as hydrogen supply Solvent naphtha enters the preparation of coal, makes full use of the synergistic effect between the arene of coal and the paraffin class of heavy oil, not only Coal conversion ratio and oil product yield can be improved, and is conducive to the coking problem of reactor in alleviation system, delays catalyst inactivation； Therefore, it is total in sweetening process in entire oily coal, it, can be farthest by inferior heavy while safe and clean utilization coal resources Oily " eating dry bleed ", but can effectively in extension system each device operation cycle, reduce production cost.

Specifically, as shown in Fig. 1, the described method comprises the following steps:

Hot high score gas in hot high score gas G1 in S10, step S3, the light oil in step S4, middle matter oil and step S7 G2 is sent into fixed bed hydrogenation system together, prepares oil product；The oil product includes gasoline, diesel oil etc..

Wherein, it is suspended-bed reactor or paste state bed reactor that the kerosene in step S2 refines reactor altogether；

Boiling bed hydrogenation tail oil in step S8 is sent to catalytic cracking alkene, aromatic device；

In addition, for operations condition in the method specifically:

In step sl, the catalyst is Ni-Co-Mo base water-soluble catalyst or Ni-Co-Mo base oil soluble catalytic Agent；The quality proportioning of the coal dust and hydrogen supply dissolvent oil is 1:1~1:3；

In step s 2, kerosene refines that the reaction temperature of reactor is 380~470 DEG C, reaction pressure is 6~20MPa, body altogether Product 0.5~2h of air speed^-1, hydrogen to oil volume ratio be 600:1~1500:1；Preferably, reaction temperature is 400~455 DEG C, reaction pressure For 6~10MPa, 0.8~1.2h of volume space velocity^-1, hydrogen to oil volume ratio be 800:1~1200:1.

In step s 4, cutting boiling range of the depressurized system tower bottom containing solid Residual oil be 420~550 DEG C, preferably 460~ 520℃。

In step s 6, hydrogenation catalyst used in fluidized bed reactor is that non-noble metal bar shaped or microspheric are catalyzed Agent, preferably Ni-Mo base microspheric catalyst；The hydrogenation conditions of the fluidized bed reactor are as follows: 8~20MPa of reaction pressure, 340~420 DEG C of reaction temperature, 0.5~2.0h of volume space velocity^-1, hydrogen-oil ratio 400:1~1000:1.

In the step s 7, high pressure hot separator directly and boiling bed system is connected, ebullating bed reactor product out directly into Enter high pressure hot separator and carry out flash separation, obtains hot high score gas and hot high score oil.

In step s 8, the mink cell focus cutting boiling range of the vacuum fractionation tower is 350~520 DEG C, and preferably cutting temperature is 360~480 DEG C.

In step s 9, using the decompressed wax oil of fractionating column side take-off in step S8 as hydrogen supply dissolvent oil, it is recycled back to step Rapid S1 carries out the preparation of coal, has a certain amount of aromatic hydrocarbons and naphthenic components in the decompressed wax oil, has preferable Hydrogen supply capacity, it can be ensured that lique faction of coal effect；In addition, gum level, asphalt content and impurity content in decompressed wax oil It is lower, in the subsequent processes for preparing coal, it can be effectively reduced the generation of follow up device coking, delay catalyst Inactivation, is conducive to extend the operation cycle of each device in system.

Correspondingly, the present invention also proposes another compound oil ingredient as hydrogen supply dissolvent oil, specially by fractionating column side line The part boiling bed hydrogenation tail oil of the decompressed wax oil of extraction and the extraction of fractionation column bottom, carries out being mixed to prepare compound oil ingredient, makees Progress coal preparation in step S1 is recycled back to for hydrogen supply dissolvent oil；Wherein, due in boiling bed hydrogenation tail oil content it is more Aromatic hydrocarbons and naphthenic components compound decompressed wax oil as hydrogen supply dissolvent oil with boiling bed hydrogenation tail oil, can be further The hydrogen supply capacity for improving compound oil ingredient is conducive to improve lique faction of coal effect；But the heavy constituent content of boiling bed hydrogenation tail oil, Impurity content is higher, in order to avoid the influence to follow up device coking, each device operating in the system of not influence to the full extent Under the premise of period, in the compound oil ingredient, the volume ratio of pressurization wax oil and boiling bed hydrogenation tail oil is 15:1-30:1.

In step slo, the fixed bed hydrogenation system is combined using fixed bed hydrogenation purification, hydrocracking unit, Or only with fixed bed hydrogenation refining plant.

Each component that the present invention generates during being refined altogether the oily coal of coal, inferior heavy oil, using corresponding processing side Method carries out subsequent working process or circular treatment, and oil product and chemicals is made, is sufficiently opened coal resources, inferior heavy oil Hair and utilization；In addition, by floating bed hydrocracking, boiling bed hydrogenation cracking, fixed bed hydrogenation, catalytic cracking system in entire technique Alkene, aromatic device are organically combined, and are constituted a complete oily coal and are refined system altogether, have given full play to each device and workshop section The advantages of, and it farthest is hydrocracked ability using suspended-bed reactor, inferior heavy oil is effectively treated, and The preparation for entering coal using the decompressed wax oil of downstream fractionation tower side take-off as hydrogen supply dissolvent oil, makes full use of the fragrance of coal Synergistic effect between hydro carbons and the paraffin class of heavy oil can not only improve coal conversion ratio and oil product yield, and be conducive to alleviate The coking problem of reactor in system, delays the inactivation of catalyst, is conducive to extend the operation cycle of each device in system, reduces Production cost.

In the present invention, the coal dust in step S1 be the lower coal of degree of coalification, including in mud coal, bituminous coal, lignite extremely Few one kind；

Inferior heavy oil in step S6 include consistency crude oil, reduced crude, decompression residuum, catalytic cracked oil pulp, deasphalted oil, At least one of visbreaker tar, coking heavy oil, shale oil, oil sands bitumen oil；Wherein, the Con. carbon of the inferior heavy oil For 10wt%~25wt%, solid content >=10g/L, toluene insolubles content is 1wt%~5wt%.It should be noted that this hair Method in bright can the inferior heavy oil effectively to above-mentioned parameter index handle, but be not limited to above-mentioned parameter index Inferior heavy oil.

In addition in step s 6, in order to improve coal conversion ratio and oil product yield, delay each reactor coking in system and urge Agent inactivation, the inferior heavy oil enter before boiling bed system, pre-process to inferior heavy oil；

Wherein the preprocessing process includes at least the removing that solid residue is carried out to inferior heavy oil, often contains in heavy oil There are certain solid impurity, including metallic particles, sandstone, catalyst fragments etc., particle diameter, which is 1-1000 μm, to be differed, In be greater than 40 μm of solid particle, be not only readily adsorbed in catalyst surface, reduce catalyst activity, lead to catalyst inactivation, And during the conveying of heavy oil and working process, accelerate the abrasion of pipeline and relevant device, result even in pipeline and The damage of equipment.Therefore, in the present invention, inferior heavy oil enters before fluidized bed reactor, by centrifugal device to inferior heavy Oil carries out the removing of solid residue, and 40 μm of solids removal will be greater than in inferior heavy oil.

In order to improve the removal efficiency to solid impurity in inferior heavy oil, the present invention change accordingly to centrifugal device Into as shown in attached drawing 2-6:

The centrifugal device includes shell 1, outer barrel 2, exocentric structure 3 and arrangement of clutch 5, and shell 1 has cavity structure, outside Bucket 2 is arranged in the cavity of shell 1, and outer barrel 2 is connect with shell 1, and the inside of said tub 2 has the cavity structure of closure, For accommodating the heavy oil component after centrifugation；Arrangement of clutch 5 is speed-reducing clutch, and the arrangement of clutch 5 is connect with shell 1, Exocentric structure 3 is configured in inside outer barrel 2, and the connection of exocentric structure 3 and the arrangement of clutch 5, exocentric structure 3 is in arrangement of clutch It is rotated under 5 drive, for inferior heavy oil to be centrifuged.

Wherein, arrangement of clutch 5 is conventional speed-reducing clutch, including first axle 51, the second axis 52, rotor, gear Group, clutch etc., the second axis 52 are hollow structure, and first axle 51 is arranged in the hollow structure, the second axis 52 and motor Rotor connection, rotor are connect by gear set with first axle 51, and clutch is connect with gear set, by clutch for clutch control come Regulate and control the relative rotation situation between first axle 51, the second axis 52, so that being able to carry out between first axle 51 and the second axis 52 same To synchronized rotation, or differential rotation in the same direction, or rotate backward each other；It is the prior art of speed-reducing clutch in view of it, herein Without repeating.

For exocentric structure 3, including middle bucket 32, interior bucket 31, the middle bucket 32, interior bucket 31 are drum knot closed at both ends Structure, for accommodating the inferior heavy oil without centrifuge separation；

The middle bucket 32 is configured in inside outer barrel 2, and through-hole 33, the through-hole 33 are provided on the side wall of the middle bucket 32 Aperture be less than or equal to 40 μm, middle bucket 32 is connect with the second axis 52 of arrangement of clutch 5, and middle bucket 32 is under the drive of the second axis 52 It is rotated；The interior bucket 31 is configured in inside middle bucket 32, and the hole that aperture is greater than 1000 μm is provided on the side wall of interior bucket 31 Structure, interior bucket 31 are connect with the first axle 51 of arrangement of clutch 5, and interior bucket 31 is rotated under the drive of first axle 51；Wherein, One axis 51, the second axis 52, middle bucket 32, interior bucket 31 are concentric setting.Preferably, every progress between middle bucket 32 and interior bucket 31 After 3 minutes rotate at the same speed in the same direction, differential rotation in the same direction in 1 minute is carried out.Corresponding outer barrel 2 is used as fixing barrel, without rotating, the Two axis 52 pass through outer barrel 2 and connects with middle bucket 32, in order to improve the leakproofness between outer barrel 2 and the second axis 52, the second axis 52 and outside It is attached between bucket 2 by bearing seal.

As shown in figures 5-6, the operational process of the centrifugal device is to put into inferior heavy oil in interior bucket 31, with The starting of arrangement of clutch 5, interior bucket 31, middle bucket 32 are rotated, and inferior heavy oil and solid matter therein are rotated with it such as Fig. 5 Shown, with interior bucket 31, the further rotation of middle bucket 32, centrifugal action is increasing, and solid matter almost all enters interior Between bucket 31 and middle bucket 32, and partial size greater than 40 μm of particle entrapment between interior bucket 31 and middle bucket 32, heavy oil by be centrifuged into Enter between middle bucket 32 and outer barrel 2 as shown in fig. 6, to realize the solid matter in inferior heavy oil is centrifuged.

As a preferred solution of the present invention, it is contemplated that accumulation situation of the solid matter in interior bucket 31, middle bucket 32, it is described in It is connected in a manner of it can dismantle between bucket 32 and the second axis 52 of arrangement of clutch 5, the first axle 51 of interior bucket 31 and arrangement of clutch 5 Between connected in a manner of it can dismantle so that in actual production use process, multiple middle buckets 32 or interior bucket 31 can be used, It is replaced and cleaning work as needed.

In addition, preferably, in order to improve the continuous operation of inferior heavy oil centrifuging treatment workshop section, the centrifugation dress Setting further includes feed pipe 6, discharge nozzle 7, and the feed pipe 6, middle bucket 32, interior bucket 31, first axle 51, the second axis 52 are concentric Setting, feed pipe 6 connect with outer barrel 2, middle bucket 32, interior bucket 31 respectively, i.e., feed pipe 6 successively extended into inside outer barrel 2 from outside, Inside middle bucket 32, inside interior bucket 31, and the batch feeding end of feed pipe 6 is arranged inside interior bucket 31；

Preferably, be connected and sealed between feed pipe 6 and outer barrel 2 or feed pipe 6 and outer barrel 2 between be integrally formed； Between feed pipe 6 and middle bucket 32, between feed pipe 6 and interior bucket 31, it is attached by bearing seal；The discharge nozzle 7 It is connect with outer barrel 2, and discharge nozzle 7 is connected to the internal cavity structures of outer barrel 2.By the way that feed pipe 6, discharge nozzle 7 is arranged, so that from Center device is able to carry out the operation of continuous feed-continuous discharge continuous centrifugal, without carrying out batch centrifugal to inferior heavy oil Operation, this undoubtedly improves centrifuge separation efficiency, alleviates productive labor intensity, advantageously reduces production cost.

Correspondingly, due to also needing to carry out separation of solid and liquid operation to containing solid Residual oil in step S5, as of the invention excellent Scheme is selected, is also centrifuged in step s 5 using above-mentioned centrifugal device to containing solid Residual oil, specifically, being walked in step S5- In the actual mechanical process of rapid S6, scheme a can be used: isolate Residual oil using centrifugal device containing solid Residual oil, inferior heavy oil makes Heavy oil is isolated with another centrifugal device, then Residual oil and heavy oil are mixed into fluidized bed reactor；Scheme can also be used B: in step s 5, inferior heavy oil is directly mixed with containing solid Residual oil, is centrifuged in centrifugal device, by the oil after separation Product put into fluidized bed reactor；Scheme c can also be used: after isolating Residual oil using centrifugal device containing solid Residual oil, by inferior heavy Oil is mixed with Residual oil, and mixture is centrifuged using centrifugal device, and the oil product after separation is put into fluidized bed reactor； Wherein, scheme c is as the preferred embodiment in step S5- step S6 actual mechanical process.

Inferior heavy oil is pre-processed by the way that centrifugal device is arranged, when can efficiently control into fluidized bed reactor The solid content of inferior heavy oil slows down the coking situation of downstream reactor, is conducive to improve coal conversion ratio and oil product yield, extends dress The operation cycle set；And for the boiling bed system in step S6, when carrying out hydrogenation reaction, catalyst is flow regime, Catalyst flowing is realized by outer or internal circulation pump, and catalyst is drawn off and added online using pressure differential method realization.Wherein, ebullated bed System includes an at least fluidized bed reactor, and preferably, boiling bed system includes more concatenated fluidized bed reactors, specifically As shown in Fig. 7, the boiling bed system includes at least three concatenated ebullated beds, wherein the first ebullated bed 91 and centrifugal device 8 are connected by discharge nozzle 7, and the top of the first ebullated bed 91 is provided with the first feeder pipe 911 and the first tandem tube 912, under first Material valve is provided in expects pipe 911 and the first tandem tube 912, the first feeder pipe 911 is connect with major ingredient pipe 10, the first series connection Pipe 912 is connect with the second ebullated bed 92；The top of second ebullated bed 92 is provided with the second feeder pipe 921 and the second tandem tube 922, Material valve is provided on second feeder pipe 921 and the second tandem tube 922, the second feeder pipe 921 is connect with major ingredient pipe 10, the Two tandem tubes 922 are connect with third ebullated bed 93；Subsequent boiling bed structure and connection relationship are boiled with the first ebullated bed 91, second It is all the same to rise bed 92, until last ebullated bed；As space is limited, in fig. 7, third ebullated bed 93 can be considered most Latter ebullated bed, the top of third ebullated bed 93 are provided with third feeder pipe 931, are provided with material on third feeder pipe 931 Valve, third feeder pipe 931 are connect with major ingredient pipe 10；Wherein, major ingredient pipe 10 is connect with the high pressure hot separator in step S7, is used It is separated in the material for passing through boiling bed hydrogenation to be delivered in high pressure hot separator.

Wherein, during boiling bed hydrogenation, if only needing an ebullated bed, the valve of the first tandem tube 912 is closed, Open the valve of the first feeder pipe 911；If desired two ebullated beds then close the first feeder pipe 911, the second tandem tube 922 valve opens the valve of the first tandem tube 912, the second feeder pipe 921；It is subsequent and so on, if desired all boilings It rises bed all to use, then only opens the feeder pipe (in fig. 7, can be considered third feeder pipe 931) of last ebullated bed, i.e., The valve of third feeder pipe 931 is only opened, the valve of remaining feeder pipe is turned off, and the valve of all tandem tubes is opened.

And in the present invention, in order to while ensuring boiling bed hydrogenation effect, utmostly extend the equipment operation period, Energy consumption is reduced, inventor focuses on to have studied the relationship of index of correlation and ebullated bed operating condition in inferior heavy oil, below by way of Related content is described in detail in experimental example:

First it should be noted that the data in following experimental examples are to be obtained by inventor by many experiments, as space is limited, A part therein is only shown in the description, and those of ordinary skill in the art can understand and implement this hair under this data Bright, remainder data all has trend identical with following experiment conclusions and can obtain identical conclusion, repeats no more hereinafter.

Experimental example 1

In experimentation of the invention, inventor find in inferior heavy oil Con. carbon and toluene insolubles content and Relationship between the two to ebullated bed operating condition and adds hydrogen effect to play large effect, not only influences oil product yield, And greatly influence the operation cycle of device, the influence especially after compared with the long running time, to final oil product yield.

Specific experiment process is as follows:

The nature parameters of 1 coal dust of table

Ash content %, Ad	6.51
		Elemental analysis, %
C_daf	75.18
		H_daf	5.22
N_daf	0.98
		S_daf	0.47
O_daf	18.15

Con. carbon and the different inferior heavy oil of toluene insolubles content and grouping are taken, is all made of in the present invention oily The method that coal refines altogether, wherein coal dust is bituminous coal, and nature parameters are as shown in table 1, remaining relevant operational parameter takes median；Simultaneously On the basis of inferior heavy oil is centrifuged, the different operating condition of ebullated bed is respectively adopted, to initial stage oil product yield And the oil product yield after device operating 90 days is detected.

As shown in Table 2, when the sum of Con. carbon and toluene insolubles content in inferior heavy oil≤14%, boiling Bed system uses an ebullated bed；The sum of Con. carbon and toluene insolubles content are greater than 14% and are less than in inferior heavy oil When 25%, boiling bed system uses two ebullated beds；The sum of Con. carbon and toluene insolubles content in inferior heavy oil >= When 25%, boiling bed system at least uses three ebullated beds.

Initial stage oil product yield in 2 each group of table and the oil product yield situation after device operating 90 days

Wherein, gasoline, diesel oil distillate quality, boiling bed hydrogenation tail oil quality are generated in the oil product yield=entire technique The sum of/(inferior heavy oil quality+dry ash free basis quality of pc+dry ash free basis catalyst carrier quality) × 100%, it is described to urge Agent carrier quality refers both to the catalyst for using coal dust as carrier.

In addition, researcher of the invention is to of the present invention a kind of for bad according to the related experiment in experimental example 1 Reduced fuel oil, coal refine altogether production oil product and chemicals method, also carried out further technological improvement, specifically to step S6 into Capable technological improvement；

Specifically, the step S6 includes:

Wherein, Con. carbon is detected according to GB 268-1987 " oil product Conradson method (converse method) ", GB/T 2292-1997 " measurement of coke chemicals toluene insolubles content " detects toluene insolubles content's index；

In addition, can also be detected to the solid content in inferior heavy oil in step S601, specifically can be used commercially available Oil product solid content detector detects solid content index.

Wherein, as a preferred solution of the present invention, be to mix inferior heavy oil with the Residual oil in step S5, to mixture into Row pretreatment；

Meanwhile as another embodiment of the present invention, only inferior heavy oil can be pre-processed, then will be located in advance Inferior heavy oil after reason is mixed with the Residual oil in step S5, and investment boiling bed system carries out plus hydrogen；

In addition, the pretreatment is to carry out the removing of solid residue to inferior heavy oil by centrifugal device 8.

Wherein, by carrying out comprehensive analysis and judgement to Con. carbon in inferior heavy oil and toluene insolubles content, bad When the sum of Con. carbon and toluene insolubles content in reduced fuel oil≤14%, boiling bed system only opens an ebullated bed；

Preferably, the first ebullated bed 91 is come into operation, the second ebullated bed 92, third ebullated bed 93 are turned off, And the valve of the first tandem tube 912 is closed, open the valve of the first feeder pipe 911.

Wherein, in inferior heavy oil when the sum of Con. carbon and toluene insolubles content >=25%, boiling bed system makes With at least three ebullated beds；Preferably, the first ebullated bed 91 in the bed system that boils, the second ebullated bed 92, third are boiled Bed 93 comes into operation, while opening the valve of third feeder pipe 931, and the valve of remaining feeder pipe is turned off, and all series connection The valve of pipe is opened.

Wherein, the sum of Con. carbon and toluene insolubles content are greater than 14% and when less than 25% in inferior heavy oil, The bed system that boils uses two ebullated beds, and is two adjacent ebullated beds；Preferably, by the first boiling in the bed system that boils Rise bed 91, the second ebullated bed 92 comes into operation, close third ebullated bed, and close the first feeder pipe 911, the second tandem tube 922 Valve, open the first tandem tube 912, the second feeder pipe 921 valve.

A specific embodiment of the invention is further described with reference to embodiments, is not therefore limited the present invention System is within the scope of the embodiment described.

Embodiment 1

S1, hydrogen supply dissolvent oil, 100 mesh coal dust below and Ni-Co-Mo base oil-soluble catalyst are hybridly prepared into oily coal Slurry, hydrogen supply dissolvent oil and coal dust are mixed in the ratio of 1:1, and the additive amount of catalyst is the 7.5% of quality of pc；Coal dust Property is as shown in table 1；

S2, the coal in step S1 is mixed with hydrogen, after preheated device preheating, into suspended-bed reactor, anti- Answer 380 DEG C of temperature, reaction pressure 20MPa, volume space velocity 0.5h^-1, carry out hydrogenation reaction under conditions of hydrogen to oil volume ratio 1500:1；

S3, the reaction product in step S2 is isolated into hot high score gas G1 and hot high score oil O1 through high pressure hot separator；Its In, the temperature of high pressure hot separator is 390 DEG C；

S4, hot high score oil O1 enter vacuum distillation tower after depressurizing and are fractionated, and isolate light oil, middle matter oil and decompression Tower tower bottom contains solid Residual oil；Wherein, the operating condition of vacuum distillation tower are as follows: 420 DEG C of column bottom temperature, tower top residual voltage 40mmHg；

S5, Residual oil and semicoke are isolated through solid-liquid separation system containing solid Residual oil；Wherein, semicoke is through gasification, Water gas shift/WGS After gas purification, it is used for hydrogen making, is used for hydrogenation reaction in device；

After the centrifugalled pretreatment of S6, inferior heavy oil, boiling bed system is mixed into the Residual oil in step S5 It carries out adding hydrogen；Wherein, solid content is 10g/L, Con. carbon 25wt% in inferior heavy oil, and toluene insolubles content is 5wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 8MPa, 420 DEG C of reaction temperature, volume space velocity 2h^-1, hydrogen-oil ratio 400:1；

Hot high score in S10, the light oil by hot high score gas G1, the step S4 in step S3, middle matter oil and step S7 Gas G2 mixing, into fixed bed hydrogenation finishing reactor；The hydrofining reaction is catalyzed using the hydrofinishing of Ni-Mo-W series Agent, 360 DEG C of reaction temperature, reaction pressure 16MPa, volume space velocity 0.35h^-1, added under conditions of hydrogen to oil volume ratio 1000:1 Hydrogen purification；

S11, the hydrotreated product in step S10 is directly entered to fixed bed hydrogenation cracker, described plus hydrogen is split Change reaction and uses Ni-W series hydrocracking catalyst, 360 DEG C of reaction temperature, reaction pressure 16MPa, volume space velocity 0.35h^-1、 Hydrocracking reaction is carried out under conditions of hydrogen to oil volume ratio 1000:1.

S12, the fractionated tower of isocrackate in step S11 is fractionated out into gasoline, diesel oil and fractionating column bottom of tower heavy oil, Fractionating column bottom of tower heavy oil is recycled back in step S11 again, enter together with the hydrotreated product hydrocracking reactor into Row hydrocracking reaction, the fractionating column bottom of tower heavy oil account for the 3% of isocrackate gross mass.

S13, the boiling bed hydrogenation tail oil in step S8 is sent to catalytic cracking alkene, aromatic device and is reacted, it is raw At light hydrocarbon gas, catalytic naphtha, catalytic diesel oil and catalytic slurry, catalytic slurry returns again to fluidized bed reactor and carries out freshening, For catalytic naphtha by fixed bed pre-hydrotreating reaction, reaction generates light hydrocarbon gas, catalytic refining naphtha and catalysis light naphthar, Catalytic refining naphtha produces benzene,toluene,xylene by Aromatics Extractive Project, raffinates oil and heavy aromatics, raffinates oil and be catalyzed pumice Cerebrol returns to catalyst cracker and carries out freshening, and catalytic diesel oil modifies production diesel oil finished product by fixed bed hydrogenation.

The coal conversion ratio at equipment operation initial stage during being refined altogether kerosene, is set the initial stage oil product yield at equipment operation initial stage Coal conversion ratio of the received shipment turn after 90 days, the oil product yield after equipment operation 90 days are detected, and the results are shown in Table 3.

Embodiment 2

After the centrifugalled pretreatment of S6, inferior heavy oil, boiling bed system is mixed into the Residual oil in step S5 It carries out adding hydrogen；Wherein, solid content is 20g/L, Con. carbon 10wt% in inferior heavy oil, and toluene insolubles content is 3wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 8MPa, 420 DEG C of reaction temperature, volume space velocity 2h^-1, hydrogen-oil ratio 400:1；

S9, decompressed wax oil, the boiling bed hydrogenation tail oil in step S8 are mixed according to volume ratio 15:1, and are recycled back to Coal preparation is carried out as hydrogen supply dissolvent oil in step S1；

S13, remaining boiling bed hydrogenation tail oil in step S8 is sent to catalytic cracking alkene, aromatic device progress instead It answers, generates light hydrocarbon gas, catalytic naphtha, catalytic diesel oil and catalytic slurry, catalytic slurry returns again to fluidized bed reactor progress Freshening, for catalytic naphtha by fixed bed pre-hydrotreating reaction, reaction generates light hydrocarbon gas, catalytic refining naphtha and catalysis pumice Cerebrol, catalytic refining naphtha produce benzene,toluene,xylene by Aromatics Extractive Project, raffinate oil and heavy aromatics, raffinate oil and be catalyzed Light naphthar returns to catalyst cracker and carries out freshening, and catalytic diesel oil modifies production diesel oil finished product by fixed bed hydrogenation.

Embodiment 3

S1, hydrogen supply dissolvent oil, 100 mesh coal dust below and Ni-Co-Mo base water-soluble catalyst are hybridly prepared into oily coal Slurry, hydrogen supply dissolvent oil and coal dust are mixed in the ratio of 2:1, and the additive amount of catalyst is the 15% of quality of pc；Coal dust Property is as shown in table 1；

S2, the coal in step S1 is mixed with hydrogen, after preheated device preheating, into suspended-bed reactor, anti- Answer 470 DEG C of temperature, reaction pressure 6MPa, volume space velocity 2h^-1, carry out hydrogenation reaction under conditions of hydrogen to oil volume ratio 600:1；

S3, the reaction product in step S2 is isolated into hot high score gas G1 and hot high score oil O1 through high pressure hot separator；Its In, the temperature of high pressure hot separator is 385 DEG C；

S4, hot high score oil O1 enter vacuum distillation tower after depressurizing and are fractionated, and isolate light oil, middle matter oil and decompression Tower tower bottom contains solid Residual oil；Wherein, the operating condition of vacuum distillation tower are as follows: 550 DEG C of column bottom temperature, tower top residual voltage 30mmHg；

S6, inferior heavy oil are mixed with the Residual oil in step S5, after common centrifugalled pretreatment, into ebullated bed System carries out plus hydrogen；Wherein, solid content is 25g/L, Con. carbon 20wt% in inferior heavy oil, and toluene insolubles content is 1wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 20MPa, 340 DEG C of reaction temperature, volume space velocity 0.5h^-1, hydrogen-oil ratio 1000:1；

Embodiment 4

S1, hydrogen supply dissolvent oil, 100 mesh coal dust below and Ni-Co-Mo base water-soluble catalyst are hybridly prepared into oily coal Slurry, hydrogen supply dissolvent oil and coal dust are mixed in the ratio of 2.5:1, and the additive amount of catalyst is the 10% of quality of pc；Coal dust Property it is as shown in table 1；

S2, the coal in step S1 is mixed with hydrogen, after preheated device preheating, into suspended-bed reactor, anti- Answer 400 DEG C of temperature, reaction pressure 8MPa, volume space velocity 1h^-1, carry out hydrogenation reaction under conditions of hydrogen to oil volume ratio 1000:1；

S4, hot high score oil O1 enter vacuum distillation tower after depressurizing and are fractionated, and isolate light oil, middle matter oil and decompression Tower tower bottom contains solid Residual oil；Wherein, the operating condition of vacuum distillation tower are as follows: 450 DEG C of column bottom temperature, tower top residual voltage 30mmHg；

After the centrifugalled pretreatment of S6, inferior heavy oil, boiling bed system is mixed into the Residual oil in step S5 It carries out adding hydrogen；Wherein, solid content is 25g/L, Con. carbon 20wt% in inferior heavy oil, and toluene insolubles content is 5wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 16MPa, 388 DEG C of reaction temperature, volume space velocity 1h^-1, hydrogen-oil ratio 600:1；

S9, the decompressed wax oil in step S8, boiling bed hydrogenation tail oil are mixed according to volume ratio 30:1, and are recycled back to step Coal preparation is carried out as hydrogen supply dissolvent oil in rapid S1；

Embodiment 5

S1, hydrogen supply dissolvent oil, 100 mesh coal dust below and Ni-Co-Mo base oil-soluble catalyst are hybridly prepared into oily coal Slurry, hydrogen supply dissolvent oil and coal dust are mixed in the ratio of 3:1, and the additive amount of catalyst is the 15% of quality of pc；Coal dust Property is as shown in table 1；

S2, the coal in step S1 is mixed with hydrogen, after preheated device preheating, into suspended-bed reactor, anti- Answer 420 DEG C of temperature, reaction pressure 12MPa, volume space velocity 1.5h^-1, carry out hydrogenation reaction under conditions of hydrogen to oil volume ratio 1200:1；

S4, hot high score oil O1 enter vacuum distillation tower after depressurizing and are fractionated, and isolate light oil, middle matter oil and decompression Tower tower bottom contains solid Residual oil；Wherein, the operating condition of vacuum distillation tower are as follows: 500 DEG C of column bottom temperature, tower top residual voltage 30mmHg；

After the centrifugalled pretreatment of S6, inferior heavy oil, boiling bed system is mixed into the Residual oil in step S5 It carries out adding hydrogen；Wherein, solid content is 25g/L, Con. carbon 20wt% in inferior heavy oil, and toluene insolubles content is 5wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 15MPa, 360 DEG C of reaction temperature, volume space velocity 1.2h^-1, hydrogen-oil ratio 800:1；

S9, the decompressed wax oil in step S8, boiling bed hydrogenation tail oil are mixed according to volume ratio 24:1, and are recycled back to step Coal preparation is carried out as hydrogen supply dissolvent oil in rapid S1；

Embodiment 6

S6, inferior heavy oil are mixed with the Residual oil in step S5, after common centrifugalled pretreatment, into ebullated bed System carries out plus hydrogen；Wherein, solid content is 25g/L, Con. carbon 20wt% in inferior heavy oil, and toluene insolubles content is 5wt%；The bed system that boils includes three concatenated fluidized bed reactors, boiling bed hydrogenation reaction condition are as follows: reaction pressure 15MPa, 360 DEG C of reaction temperature, volume space velocity 1.2h^-1, hydrogen-oil ratio 800:1；

Comparative example 1

Oily coal is carried out using the technical solution of embodiment 2 in CN106433775A to refine altogether, specifically:

Coal is crushed to 3mm hereinafter, then drying to it makes its moisture be down to < 3% hereinafter, using ball again by crusher It is spare that grinding machine is milled to 100 mesh or less.In mink cell focus preprocessing process, reaction temperature is 410 DEG C, reaction pressure 16MPa, Gas liquid ratio is 1000, and atmospheric resid feed amount is 8kg/h, catalyst loading 1%.Heavy distillate and coal dust are configured to The coal of coal powder density 40%, the inlet amount of coal are 8kg/h, at 450 DEG C of reaction temperature, reaction pressure 19MPa, gas-liquid Coprocessing reaction is carried out under the conditions of than 1500.Wherein, the property of coal dust is as shown in table 1；Solid content is 25g/L, health in mink cell focus Family name's carbon residue is 20wt%, and toluene insolubles content is 5wt%.

Comparative example 2

Operating process, operating condition and operating parameter in comparative example 2 is same as Example 6, the difference is that in step In rapid S6, comparative example 2 is not pre-processed inferior heavy oil, and the Residual oil in inferior heavy oil and step S5 is directly mixed into boiling Bed system is risen to carry out adding hydrogen.

In 3 embodiment of table and comparative example the case where related coal conversion ratio, oil product yield

Wherein, coal conversion ratio=1- (in solid residue quality-coal dust in moisture and ash content quality-catalyst moisture and Ash content quality)/(dry ash free basis quality of pc+dry ash free basis catalyst carrier quality) × 100%；

Oil product yield=(quality of gasoline+diesel oil distillate quality+boiling bed hydrogenation tail oil quality is generated in entire technique)/ (inferior heavy oil quality+dry ash free basis quality of pc+dry ash free basis catalyst carrier quality) × 100%；The catalyst Carrier quality refers both to the catalyst for using coal dust as carrier.

By the data in table 3 it is found that coal conversion ratio and oil product yield of the embodiment 1-4 at equipment operation initial stage, compared to pair Ratio 1-2 is improved in the coal conversion ratio and oil product yield at equipment operation initial stage, and has statistical significance (p < 0.01).

In addition, the coal conversion ratio and oil product yield of bonding apparatus start of run are analyzed, embodiment 1-4 is in equipment operation The index fall of coal conversion ratio and oil product yield after 90 days, coal of the respectively less than ratio 1-2 after equipment operation 90 days turn The index fall (p < 0.01) of rate and oil product yield, this illustrates that the method in the present invention can effectively alleviate system Coking problem has delayed the inactivation of catalyst, extends the operation cycle of production equipment.

In embodiment 2, embodiment 4-5, uses decompressed wax oil and mixed with part boiling bed hydrogenation tail oil as hydrogen supply The embodiment of solvent naphtha, can as seen from Table 3, and coal conversion ratio has small size raising, although after equipment operation 90 days The index fall of coal conversion ratio and oil product yield is all larger than other embodiments, but still in a better index model Enclose (p < 0.01)；And embodiment 2, embodiment 4-5 all indicators are better than comparative example 1-2 (p < 0.01), this also illustrates this The method of invention and relevant embodiment are avoiding not influencing the influence of follow up device coking to the full extent as far as possible In system under the premise of each device operation cycle, coal conversion ratio is further improved.

Further, either the coal conversion ratio and oil product yield at equipment operation initial stage or after equipment operation 90 days The index fall of coal conversion ratio and oil product yield, comparative example 2 are better than the index of correlation (p < 0.01) of comparative example 1, but Obviously it is inferior to embodiment 1-4 (p < 0.01), this illustrates that the method in the present invention, each step are all indispensable, and these are made The combination of standby step can obtain unexpected technical effect.

The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims

1. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal, which is characterized in that coal dust, hydrogen supply is molten Agent oil and catalyst are mixed with coal, refine in reactor and crack altogether in kerosene, hot high score oil isolated to pyrolysis product O1 carries out vacuum fractionation to hot high score oil O1 and obtains to contain solid Residual oil containing solid Residual oil and being separated by solid-liquid separation to obtain Residual oil；It will be inferior Heavy oil is blended in fluidized bed reactor with Residual oil and is hydrocracked, hot high score oil O2 isolated to crackate, to hot high score Oily O2 carries out vacuum fractionation and is recycled into oil for decompressed wax oil as hydrogen supply dissolvent oil in fractionating column side take-off decompressed wax oil The preparation of coal slurry.

2. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as described in claim 1, feature exist In the coal dust includes at least one of mud coal, bituminous coal, lignite；

The inferior heavy oil include consistency crude oil, reduced crude, decompression residuum, catalytic cracked oil pulp, deasphalted oil, visbreaker tar, At least one of coking heavy oil, shale oil, oil sands bitumen oil；

Wherein, solid content >=10g/L of the inferior heavy oil, Con. carbon are 10wt%~25wt%, and toluene insolubles contain Amount is 1wt%~5wt%.

3. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as described in claim 1, feature exist In, comprising the following steps:

S3, kerosene refine the reaction product in reactor altogether, separate through high pressure hot separator, obtain hot high score gas G1 and hot high score oil O1；

Hot high score oil O1 in S4, step S3 enters decompression distillation system and is fractionated, and isolates light oil, middle matter oil, containing solid Residual oil；

S7, fluidized bed reactor reaction product are separated through high pressure hot separator, obtain hot high score gas G2 and hot high score oil O2；

Hot high score oil O2 in S8, step S7, which is sent to vacuum fractionation tower, to be separated, in fractionating column side take-off decompressed wax oil, Fractionation column bottom produces boiling bed hydrogenation tail oil；

Hot high score gas G2 mono- in hot high score gas G1 in S10, step S3, the light oil in step S4, middle matter oil and step S7 It rises and is sent into fixed bed hydrogenation system, prepare oil product.

4. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature exist In in the method, the boiling bed hydrogenation tail oil in step S8 is sent to catalytic cracking alkene, aromatic device；

Semicoke in step S5 is Filter Tuber For Clean Coal, can sell, also be able to enter Hydrogen Unit, through gasification, Water gas shift/WGS, Hydrogen is produced in gas purification, refines reactor, the boiling bed system in step S6 altogether, in step S10 for the kerosene in step S2 Fixed bed hydrogenation system use.

5. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature exist In in step s 6, inferior heavy oil enters before fluidized bed reactor, pre-processes to inferior heavy oil.

6. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 5, feature exist In the pretreatment is to carry out the removing of solid residue to inferior heavy oil by centrifugal device (8), and 40 will be greater than in inferior heavy oil μm solids removal.

7. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature exist In the boiling bed system includes at least three concatenated ebullated beds；

First ebullated bed (91) and centrifugal device (8) are connect by discharge nozzle (7), and the top of the first ebullated bed (91) is provided with the Material is provided on one feeder pipe (911) and the first tandem tube (912), the first feeder pipe (911) and the first tandem tube (912) Valve, the first feeder pipe (911) are connect with major ingredient pipe (10), and the first tandem tube (912) is connect with the second ebullated bed (92)；

The top of second ebullated bed (92) is provided with the second feeder pipe (921) and the second tandem tube (922), the second feeder pipe (921) and on the second tandem tube (922) it is provided with material valve, the second feeder pipe (921) is connect with major ingredient pipe (10), and second Tandem tube (922) is connect with third ebullated bed (93)；

The top of third ebullated bed (93) is provided with third feeder pipe (931), and third feeder pipe is provided with Material valve on (931) Door, third feeder pipe (931) are connect with major ingredient pipe (10)；

Major ingredient pipe (10) is connect with the high pressure hot separator in step S7, for the material for passing through boiling bed hydrogenation to be delivered to heat It is separated in high-pressure separator.

8. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature exist In step S6 includes:

S605, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein a boiling is used only in boiling bed system Rise bed；

S606, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein boiling bed system at least uses three Ebullated bed；

S607, mixture after pretreatment investment boiling bed system carries out plus hydrogen, wherein boiling bed system uses two boilings Bed.

9. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature exist In in step sl, the catalyst is Ni-Co-Mo base water-soluble catalyst or Ni-Co-Mo base oil-soluble catalyst；It is described The quality proportioning of coal dust and hydrogen supply dissolvent oil is 1:1~1:3.

10. a kind of method for refining production oil product and chemicals altogether for inferior heavy oil, coal as claimed in claim 3, feature It is, in step s 2, it is suspended-bed reactor or paste state bed reactor that the kerosene refines reactor altogether；Kerosene refines reactor altogether Reaction temperature be 380~470 DEG C, reaction pressure is 6~20MPa, 0.5~2h of volume space velocity^-1, hydrogen to oil volume ratio 600:1 ~1500:1；

In step s 6, the hydrogenation conditions of the fluidized bed reactor are as follows: 8~20MPa of reaction pressure, reaction temperature 340 ~420 DEG C, 0.5~2.0h of volume space velocity^-1, hydrogen-oil ratio 400:1~1000:1.