CN108048121A - Coal direct liquefaction method and Direct coal liquefaction device - Google Patents

Coal direct liquefaction method and Direct coal liquefaction device Download PDF

Info

Publication number
CN108048121A
CN108048121A CN201711203668.6A CN201711203668A CN108048121A CN 108048121 A CN108048121 A CN 108048121A CN 201711203668 A CN201711203668 A CN 201711203668A CN 108048121 A CN108048121 A CN 108048121A
Authority
CN
China
Prior art keywords
liquefaction
coal
product
direct
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711203668.6A
Other languages
Chinese (zh)
Other versions
CN108048121B (en
Inventor
高山松
舒歌平
李克健
杨葛灵
章序文
李永伦
王洪学
姜元博
王国栋
杨玉峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Group Corp Ltd
Shanghai Research Institute of China Shenhua Coal to Liquid Chemical Co Ltd
Original Assignee
China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Group Corp Ltd
Shanghai Research Institute of China Shenhua Coal to Liquid Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Shenhua Coal to Liquid Chemical Co Ltd, Shenhua Group Corp Ltd, Shanghai Research Institute of China Shenhua Coal to Liquid Chemical Co Ltd filed Critical China Shenhua Coal to Liquid Chemical Co Ltd
Priority to CN201711203668.6A priority Critical patent/CN108048121B/en
Publication of CN108048121A publication Critical patent/CN108048121A/en
Application granted granted Critical
Publication of CN108048121B publication Critical patent/CN108048121B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/006Combinations of processes provided in groups C10G1/02 - C10G1/08
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70Catalyst aspects
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2400/00Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/04Diesel oil

Abstract

The present invention provides a kind of coal direct liquefaction method and Direct coal liquefaction devices.The coal direct liquefaction method comprises the following steps:S1 makes the first raw material for including coal slurry and hydrogen carry out first time liquefaction reaction, obtains the first liquefaction products, and carries out Oil-gas Separation to the first liquefaction products, obtains the first liquid product;S2 makes the second raw material for including the first liquid product, hydrogen and solvent carry out second of liquefaction reaction, obtains the second liquefaction products, and carries out Oil-gas Separation to the second liquefaction products, obtains second liquid phase product;S3, distills part second liquid phase product and catalytic hydrogenation treatment, obtains Coal Liquefaction Products;And S4, above-mentioned steps S1 is repeated to S3, and the first raw material and/or the second raw material further include remainder second liquid phase product during repeating.Lique faction of coal conversion ratio and liquid product yield can be improved using above-mentioned coal direct liquefaction method, resource utilization is obviously improved.

Description

Coal direct liquefaction method and Direct coal liquefaction device
Technical field
The present invention relates to coal chemical technology, in particular to a kind of coal direct liquefaction method and Direct coal liquefaction device.
Background technology
Direct coal liquefaction technology refer to coal in high temperature, high pressure, face hydrogen, solvent and catalyst under the action of, it is straight by being hydrogenated with Connect the technical process for being converted into fluid product and a small amount of gas products.Direct coal liquefaction process process generally includes four mainly Part:Coal preparation, Coal Liquefaction reaction, separation of solid and liquid and product upgrading processing and utilization.Coal wears into coal through broken drying Powder, be configured to together with solvent, catalyst be suitble to conveying and heat transfer coal, coal it is boosted and preheating after be delivered to coal Hydrogenation liquefaction reactor, the product of pyrolysis and hydrogenation reaction generation liquid occurs for coal under conditions of high temperature and pressure, and reaction is given birth to Into liquefaction oil separated with bitumen, unconverted coal, catalyst and ash content, recycling design obtains coal liquefaction crude oil, Coal liquefaction crude oil is subjected to upgrading processing target product again, the scheme difference according to product can produce gasoline, diesel oil, aviation Kerosene, specialty oil and industrial chemicals etc..
The current main influence for influencing DCL/Direct coal liquefaction realization industrialization includes Installed capital cost height, lique faction of coal conversion Rate and oil yield are low, wherein the low economic benefit for being the most key factor, directly affecting Direct coal liquefaction device of oil yield And the market competitiveness.Since direct coal liquefaction process condition is comparatively harsh, Coal liquefaction temperature is higher, DCL/Direct coal liquefaction Reaction process mainly includes pyrolysis and hydrogenation, unavoidably causes the second pyrolysis of target product, causes target product oil yield It reduces, bi-product gas yield is high, while also increases hydrogen consumption, cost increase;In addition, during Coal liquefaction, coal Activearm component convert first, it is difficult to the component of conversion then needs more harsh conditions, and DCL/Direct coal liquefaction was reacted Journey is a parallel series reaction system, this also causes the second half in second reactor or reaction, cycles the confession Hydrogen Energy of solvent Power declines, and hydrogen partial pressure reduces, and reaction severity reduces instead, this is unfavorable for improving lique faction of coal conversion ratio and oil yield.Currently DCL/Direct coal liquefaction reaction process is a parallel series reaction system in the anti-technique of most DCL/Direct coal liquefaction, thus is had The problem of like above.
Therefore, in the case where equipment investment amplification is little, reach effective there is an urgent need for developing DCL/Direct coal liquefaction new process at present Gas yield and hydrogen consumption are reduced, improves lique faction of coal conversion ratio, realizes the purpose for increasing oil yield, is conducive to improve the utilization of resources Rate enhances DCL/Direct coal liquefaction economic benefit and the market competitiveness.
The content of the invention
It is existing to solve it is a primary object of the present invention to provide a kind of coal direct liquefaction method and Direct coal liquefaction device The relatively low gentle yield of coal direct liquefaction method liquefying conversion rate in technology is higher, so as to cause oil yield it is poor the problem of.
To achieve these goals, according to an aspect of the invention, there is provided a kind of coal direct liquefaction method, including with Lower step:S1 makes the first raw material for including coal slurry and hydrogen carry out first time liquefaction reaction, obtains the first liquefaction products, and right First liquefaction products carry out Oil-gas Separation, obtain the first liquid product;S2 makes to include the first liquid product, hydrogen and solvent Second raw material carries out second of liquefaction reaction, obtains the second liquefaction products, and carries out Oil-gas Separation to the second liquefaction products, obtains Second liquid phase product;S3, distills part second liquid phase product and catalytic hydrogenation treatment, obtains Coal Liquefaction Products;And S4 repeats above-mentioned steps S1 to S3, and the first raw material and/or the second raw material further include residue during repeating Part second liquid phase product.
Further, the inlet amount of remainder second liquid phase product and the first raw material is than 0.1~1, remainder second The inlet amount of liquid product and the second raw material is than 0.1~1.
Further, the pressure of first time liquefaction reaction and/or second of liquefaction reaction be each independently 15~ 20MPa, reaction temperature are each independently 440~460 DEG C, and the volume of hydrogen and the weight ratio of coal slurry are each independently 800~1200L/Kg.
Further, coal slurry includes coal dust and catalyst for coal liquefaction, and preferably catalyst for coal liquefaction includes nanoscale hydration oxygen Change any one of iron, natural crystal, the compound of pure state iron and nanoscale ferrous sulfide or a variety of, more preferable coal liquefaction catalysis Agent is nanoscale hydrated ferric oxide;It is preferred that the dosage of catalyst for coal liquefaction accounts for 0.5~1.5wt% of coal slurry.
Further, in step sl, the temperature for the first liquefaction products being carried out with Oil-gas Separation is 410~440 DEG C, the time Less than 5min, the preferably time is less than 3min.
Further, in step s 2, the temperature for the second liquefaction products being carried out with Oil-gas Separation is 380~430 DEG C.
Further, in step s3, the pressure of catalytic hydrogenation treatment is 15~19MPa, and reaction temperature is 350~390 DEG C, volume space velocity is 0.8~2.0h-1, hydrogen-oil ratio is 300~800.
Further, in step s3, catalytic hydrogenation is carried out to the second liquid phase product after distillation using hydrogenation catalyst Processing, hydrogenation catalyst is loaded catalyst, and preferred vector is aluminium oxide, and the active metal component of loaded catalyst is Any one of group vib or VIII group are a variety of, and the metal component of more preferable group vib is Mo and W, and the metal component of VIII group is Ni and Co.
Further, Xun Huan solvent is also obtained in the step of carrying out catalytic hydrogenation treatment to part second liquid phase product, During repeating, the first raw material includes partly cycling solvent, and the solvent in the second raw material cycles molten for another part Agent, preferred cycle solvent are more than 220 DEG C of distillate for temperature, and density is 0.92~0.99g/cm3
Further, the first gas-phase product is obtained in the step of carrying out Oil-gas Separation to the first liquefaction products, and right Second liquefaction products carry out obtaining the second gas-phase product in the step of Oil-gas Separation, and step S3 further includes procedure below at this time:It is right The mixture of first gas-phase product and the second gas-phase product carries out Oil-gas Separation, obtains the 3rd liquid product;3rd liquid phase is produced Object is distilled and catalytic hydrogenation treatment, and preferably the mixture of the 3rd liquid product and second liquid phase product is distilled and urged Change hydrotreating.
According to another aspect of the present invention, a kind of Direct coal liquefaction device is provided, Direct coal liquefaction device includes:First Liquefying reactor has first circulation material inlet and the first product exit;Intermediate separator has the first product inlet and the One liquid-phase outlet, the first product inlet are connected with the first product exit;Second liquefying reactor has the second feed(raw material)inlet, the Two recycle stock entrances and the second product exit, the second feed(raw material)inlet are connected with the first liquid-phase outlet;First high pressure hot separator, Exported with the second product inlet and second liquid phase, the second product inlet connect with the second product exit, second liquid phase export and First circulation material inlet is connected with second circulation material inlet;There is vacuum distillation tower destilling tower entrance, destilling tower oil phase to go out Mouth and destilling tower solid-phase outlet, destilling tower entrance and second liquid phase outlet;And solvent catalysis hydrogenation unit, with destilling tower Oil phase outlet.
Further, above-mentioned intermediate separator also has the first gaseous phase outlet, and the first high pressure hot separator also has second Gaseous phase outlet, Direct coal liquefaction device further include the first cold high pressure separator, and the first cold high pressure separator respectively with the first gas Mutually outlet, the second gaseous phase outlet are connected with vacuum distillation tower entrance.
Further, above-mentioned first liquefying reactor and the second liquefying reactor are anti-independently selected from forced circulation suspension bed Device, bubbling bed reactor, paste state bed reactor and the circulation flow reactor with guide shell are answered, is preferably that forced circulation suspension bed is anti- Answer device.
Further, above-mentioned solvent catalysis hydrogenation unit includes the surge tank of sequential communication and catalytic hydrogenation reaction device, and Surge tank is connected with vacuum distillation tower, preferred catalytic hydrogenation reactor be fixed bed reactors or fluidized bed reactor, more preferably For fluidized bed reactor.
It applies the technical scheme of the present invention, provides a kind of coal direct liquefaction method, DCL/Direct coal liquefaction reaction process is drawn It is divided to two relatively independent reaction systems, due to increasing between first time liquefaction reaction and second of liquefaction reaction to for the first time Liquefaction products carry out the step of Oil-gas Separation, so as to not only significantly reduce the light oil residence time, avoid secondary cracking Problem, reduce gas yield and hydrogen consumption, also help reduce second of liquefaction reaction in gas delay, and then improve it is more difficult The residence time of transformation substance in the reaction, add the hydrogen partial pressure in reaction process;Also, due to anti-in the above-mentioned liquefaction of repetition In the step of answering, the first raw material and/or the second raw material is made to further include the second liquid that the second liquefaction products obtain after Oil-gas Separation Phase product, it is achieved thereby that cycling of the high score material in direct coal liquefaction process, the catalyst improved in liquefaction reaction contain Amount and the reaction time for being relatively difficult to convert coal and bitumen, and then lique faction of coal conversion ratio is improved, finally carry The oil yield of the high Coal Liquefaction Products obtained through catalytic hydrogenation treatment, resource utilization are obviously improved, and it is direct to enhance coal The competitiveness of liquefaction technology.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages. Below with reference to figure, the present invention is described in further detail.
Description of the drawings
The Figure of description for forming the part of the present invention is used for providing a further understanding of the present invention, and of the invention shows Meaning property embodiment and its explanation do not constitute improper limitations of the present invention for explaining the present invention.In the accompanying drawings:
Fig. 1 shows a kind of structure diagram for Direct coal liquefaction device that embodiment of the present invention is provided.
Wherein, above-mentioned attached drawing is marked including the following drawings:
110th, coal preparing tank;120th, heating furnace;130th, the first liquefying reactor;140th, intermediate separator;150th, Two liquefying reactors;160th, the first high pressure hot separator;170th, the first cold high pressure separator;180th, vacuum distillation tower;210th, delay Rush tank;220th, catalytic hydrogenation reaction device;230th, the second high pressure hot separator;240th, the second cold high pressure separator;250th, fractionating column; 101st, high-pressure coal pulp pump;102nd, coal liquefaction second reactor feed pump;103rd, hydrogenating materials pump.
Specific embodiment
It should be noted that in the case where there is no conflict, the feature in embodiment and embodiment in the present invention can phase Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
In order to which those skilled in the art is made to more fully understand the present invention program, below in conjunction in the embodiment of the present invention The technical solution in the embodiment of the present invention is clearly and completely described in attached drawing, it is clear that described embodiment is only The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people Member's all other embodiments obtained without making creative work should all belong to the model that the present invention protects It encloses.
It should be noted that term " first " in description and claims of this specification and above-mentioned attached drawing, " Two " etc. be the object for distinguishing similar, without being used to describe specific order or precedence.It should be appreciated that it so uses Data can exchange in the appropriate case, so as to the embodiment of the present invention described herein.In addition, term " comprising " and " tool Have " and their any deformation, it is intended that cover it is non-exclusive include, for example, containing series of steps or unit Process, method, system, product or equipment are not necessarily limited to those steps or unit clearly listed, but may include without clear It is listing to Chu or for the intrinsic other steps of these processes, method, product or equipment or unit.
As background technology is described, existing overwhelming majority direct coal liquefaction process methods, there are secondary cracking, The situation that gas yield and hydrogen consumption height and coal liquefaction second reactor severity reduce, oil low so as to cause lique faction of coal conversion ratio Yield is low.To solve the above-mentioned problems, the present invention provides a kind of coal direct liquefaction method, comprise the following steps:S1 makes to include First raw material of coal slurry and hydrogen carries out first time liquefaction reaction, obtains the first liquefaction products, and the first liquefaction products are carried out Oil-gas Separation obtains the first liquid product;S2 makes the second raw material for including the first liquid product, hydrogen and solvent carry out second Secondary liquefaction reaction obtains the second liquefaction products, and carries out Oil-gas Separation to the second liquefaction products, obtains second liquid phase product;S3, Part second liquid phase product is distilled and catalytic hydrogenation treatment, obtain Coal Liquefaction Products;And S4, repeat above-mentioned step Rapid S1 is to S3, and the first raw material and/or the second raw material further include remainder second liquid phase product during repeating.
In above-mentioned coal direct liquefaction method provided by the present invention, due to liquefying in first time liquefaction reaction and second Increase the step of Oil-gas Separation is carried out to the first liquefaction products between reaction, Coal liquefaction is divided into two by a system Relatively independent reaction system so as to not only significantly reduce the light oil residence time, avoids secondary cracking problem, reduces gas Body yield and hydrogen consumption, also help the delay for reducing gas in second of liquefaction reaction, and then improve more difficult transformation substance and exist Residence time in reaction adds the hydrogen partial pressure in reaction process;Also, due to repeat above-mentioned liquefaction reaction the step of In, the first raw material and/or the second raw material is made to further include the second liquid phase product that the second liquefaction products obtain after Oil-gas Separation, from And cycling of the high score material in direct coal liquefaction process is realized, improve catalyst content in liquefaction reaction and more difficult To convert the reaction time of coal and bitumen, and then lique faction of coal conversion ratio is improved, finally improved through catalysis The oil yield for the Coal Liquefaction Products that hydrotreating obtains, improves the level of resources utilization, enhances the competing of direct coal liquefaction technology Strive power.
In coal direct liquefaction method provided by the present invention, the second gas is obtained after carrying out Oil-gas Separation to the second liquefaction products Phase product (gas phase portion) and second liquid phase product (liquid-solid phase part), during above-mentioned steps S1 to S3 is repeated One raw material and/or the second raw material further include part second liquid phase product, and another part obtains liquefied coal coil and residue after distillation. Preferably, the second liquefaction products is controlled to carry out the temperature of Oil-gas Separation as 380~430 DEG C;Also, remainder second liquid phase produces The inlet amount of object and the first raw material is than 0.1~1, and the inlet amount of remainder second liquid phase product and the second raw material is than 0.1~1. By controlling above-mentioned inlet amount than can more effectively improve the catalyst content in liquefaction reaction and relatively be difficult to convert coal With the residence time of bitumen, so as to improve lique faction of coal conversion ratio and oil yield.
Those skilled in the art may be employed in coal direct liquefaction method provided by the present invention, during liquefaction reaction to exist Common catalyst during DCL/Direct coal liquefaction.In a preferred embodiment, the catalysis used during liquefaction reaction Agent is water synthesis nano hydrated ferric oxide.Using hydrated ferric oxide as the catalyst of liquefaction reaction, production cost is low, and liquefaction is lived Property it is high, catalyst loading can be reduced, improve the reaction rate of liquefaction reaction, promote the conversion of coal, improve oil yield, improved The economy of the technique reduces coal liquefaction residue amount.In addition, those skilled in the art can select the specific use of the catalyst Amount.Preferably, the dosage of above-mentioned catalyst is 0.5~1.5wt% of dry coal weight.
In coal direct liquefaction method provided by the present invention, liquefaction reaction process may be employed common in coal liquefaction Process conditions.In a preferred embodiment, the pressure of first time liquefaction reaction and/or second of liquefaction reaction can be each From 15~20MPa independently is, reaction temperature is 440~460 DEG C, and second of liquefaction reaction temperature should be with first time liquefaction reaction Temperature is identical or slightly higher, and the ratio of hydrogen and coal is 800~1200L/kg.By each process regulation of liquefaction reaction upper Scope is stated, Installed capital cost can be reduced, and Coal liquefaction can be made more abundant, there is higher coal during guarantee liquefaction reaction Conversion ratio and liquid fuel yield.
In coal direct liquefaction method provided by the present invention, increase between first time liquefaction reaction and second of liquefaction reaction Add and Oil-gas Separation is carried out to the first liquefaction products, Coal liquefaction is divided into two relatively independent reactants by a system System, the first liquefaction products are carried out with the temperature of Oil-gas Separation needs as far as possible close to the temperature of first time liquefaction reaction.A kind of excellent In the embodiment of choosing, the first liquefaction products are carried out with the temperature of Oil-gas Separation for 410~440 DEG C, the liquid phase residence time is less than 5 Minute, it is preferably less than 3 minutes, while the note disturbance measures such as hydrogen or cooling oil (cycling solvent) can be used, it can effectively control object There is a situation where cokings during Oil-gas Separation for material.
In coal direct liquefaction method provided by the present invention, Xun Huan solvent catalysis hydrogenation process may be employed oil refining industry and urge Change the process conditions of hydrogenation process.In a preferred embodiment, in above-mentioned steps S3, the pressure of catalytic hydrogenation treatment For 15~19MPa, reaction temperature is 350~390 DEG C, and volume space velocity is 0.8~2.0h-1, hydrogen-oil ratio is 300~800.It will Xun Huan Each process regulation within the above range, is conducive to catalytic hydrogenation reaction and more fully carries out in solvent catalysis hydrogenation process, The hetero atom in liquefied coal coil is removed, realizes that aromatic hydrocarbons obtains fractional saturation in liquefied coal coil, increases reactive hydrogen quantity in solvent, carries The hydrogen supply capacity of high circulation solvent produces qualified coal liquefaction Xun Huan solvent, is conducive to DCL/Direct coal liquefaction reaction, promotes coal Liquefaction conversion can relatively be fully converted into the oil of small molecule.
In coal direct liquefaction method provided by the present invention, using hydrogenation catalyst to the second liquid of part after including distillation The liquefied coal coil of phase product carries out catalytic hydrogenation treatment, and above-mentioned hydrogenation catalyst can be loaded catalyst.Add to improve Hydrogen catalyst prepares high liquefying activity Xun Huan solvent, it is preferable that carrier is aluminium oxide, load to the catalytic performance of liquefied coal coil The active metal component of type catalyst is any one of group vib or VIII group or a variety of, it is further preferable that the metal of group vib Component is Mo and W, and the metal component of VIII group is Ni and Co.
In coal direct liquefaction method provided by the present invention, to including coal liquefaction obtained by the second liquid phase product distillation of part Oil carries out also obtaining Xun Huan solvent in the step of catalytic hydrogenation treatment, and during repeating, the first raw material includes part Solvent is cycled, the solvent in the second raw material cycles solvent for another part, that is, directly adds when configuring coal using solvent catalysis Liquid be fractionated in hydrogen liquid product, in addition to liquid fuel is as Xun Huan solvent.By liquefying at second Hydrogen and Xun Huan hydrogen supply dissolvent are injected in reaction, improves the hydrogen partial pressure and active amt in reaction process, promotion is difficult to turn The coal of change and the conversion of pitch metallic substance are favourable.
In a preferred embodiment, coal liquefaction Xun Huan solvent is above-mentioned catalytic hydrogenation liquid product>220 DEG C evaporate Divide oil, density is 0.92~0.99g/cm3.Fractional saturation arene content is higher in the distillate, and hydrogen supply capacity is strong, is made with it To cycle solvent, the effect of liquefaction reaction can be further improved, and then improves the yield of liquid fuel.It is it is highly preferred that above-mentioned The density of distillate is 0.95~0.97g/cm3, total arene content>70wt%, monocyclic and two ring aromatic content>55wt%.With It is as Xun Huan solvent, and hydrogen supply capacity is stronger, the yield higher of liquid fuel.
In coal direct liquefaction method provided by the present invention, in the step of carrying out Oil-gas Separation to the first liquefaction products To the first gas-phase product, and the second gas-phase product is obtained in the step of carrying out Oil-gas Separation to the second liquefaction products, this time step Rapid S3 can also include procedure below:Oil-gas Separation is carried out to the mixture of the first gas-phase product and the second gas-phase product, is obtained 3rd liquid product;3rd liquid product is distilled and catalytic hydrogenation treatment, preferably to the 3rd liquid product and the second liquid The mixture of phase product is distilled and catalytic hydrogenation treatment.3rd liquid product and second liquid phase product are mixed and distilled To liquefied coal coil, catalytic hydrogenation treatment is carried out to it, removes the hetero atom in liquefied coal coil, realizes that aromatic hydrocarbons obtains in liquefied coal coil Fractional saturation increases reactive hydrogen quantity in solvent, and make cycling solvent has hydrogen supply capacity, is conducive to DCL/Direct coal liquefaction reaction, Promote lique faction of coal conversion, can more fully convert the oil of small molecule.
According to further aspect of the application, a kind of Direct coal liquefaction device is provided, as shown in Figure 1, DCL/Direct coal liquefaction Device includes:First liquefying reactor 130 has the first feed(raw material)inlet, first circulation material inlet and the first product exit;In Between separator 140, there is the first product inlet and the first liquid-phase outlet, the first product inlet connects with the first product exit;The Two liquefying reactors 150 have the second feed(raw material)inlet, second circulation material inlet and the second product exit, the second feed(raw material)inlet It is connected with the first liquid-phase outlet;There is first high pressure hot separator 160 second product inlet and second liquid phase to export, the second production Object entrance is connected with the second product exit, and second liquid phase outlet connects with first circulation material inlet and second circulation material inlet It is logical;Vacuum distillation tower 180 has destilling tower entrance, the outlet of destilling tower oil phase and destilling tower solid-phase outlet, destilling tower entrance and institute State second liquid phase outlet;And solvent catalysis hydrogenation unit, with destilling tower oil phase outlet.
In above-mentioned Direct coal liquefaction device provided by the present invention, due to anti-in the first liquefying reactor and the second liquefaction It answers and adds an intermediate separator between device, when being stopped so as to not only significantly reduce light oil using the intermediate separator Between, it avoids secondary cracking problem, reduces gas yield and hydrogen consumption, also help and reduce the stagnant of gas in second of liquefaction reaction It stays, and then improves the residence time of more difficult transformation substance in the reaction, add the hydrogen partial pressure in reaction process;Also, by In the second liquid phase outlet of the first high pressure hot separator and the first circulation material inlet and the second liquid of the first liquefying reactor Change the second circulation material inlet connection of reactor, it is achieved thereby that cycling of the high score material in direct coal liquefaction process, carries Catalyst content in high liquefaction reaction and the reaction time for being relatively difficult to convert coal and bitumen, and then improve Lique faction of coal conversion ratio, finally improves the oil yield of the Coal Liquefaction Products obtained through catalytic hydrogenation treatment, improves resource Utilization ratio enhances the competitiveness of direct coal liquefaction technology..
In above-mentioned Direct coal liquefaction device provided by the present invention, make to include the first raw material of coal slurry and hydrogen into the First time liquefaction reaction is carried out in one liquefying reactor 130, obtains the first liquefaction products, and using intermediate separator 140 to the One liquefaction products carry out Oil-gas Separation, obtain the first gas-phase product and the first liquid product, the operation temperature of intermediate separator 140 Need access to 130 temperature of the first liquefying reactor.In a preferred embodiment, the operation temperature of intermediate separator 140 For 410~440 DEG C, the liquid phase residence time is less than 5 minutes, is preferably less than 3 minutes, while note disturbance hydrogen or cooling oil can be used The measures such as solvent are cycled, it can effectively there is a situation where cokings in intermediate separator for control material.
In above-mentioned Direct coal liquefaction device provided by the present invention, the second raw material including the first liquid product and hydrogen Second of liquefaction reaction is carried out in the second liquefying reactor 150, obtains the second liquefaction products, the first high pressure hot separator 160 Oil-gas Separation is carried out to above-mentioned second liquefaction products, obtains the second gas-phase product gas phase portion and second liquid phase product liquid-solid phase portion Point, a second liquid phase product part is recycled in the first liquefying reactor 130 or/and the second liquefying reactor 150, another part Liquefied coal coil and residue are obtained after the distillation of vacuum distillation tower 180;In a preferred embodiment, the first thermal high separates The temperature control of device 160 is 380~430 DEG C, the ratio between liquid-solid phase solid circulating rate and coal liquefaction feedstock amount 0.1~1.
In Direct coal liquefaction device provided by the present invention, intermediate separator 140 also has the first gaseous phase outlet, the first heat High-pressure separator 160 also has the second gaseous phase outlet, and Direct coal liquefaction device further includes the first cold high pressure separator 170, and the One cold high pressure separator 170 connects respectively with the first gaseous phase outlet, the second gaseous phase outlet and vacuum distillation tower entrance.Using above-mentioned First cold high pressure separator 170 can be by the light components in the first liquefaction products and the second liquefaction products and the first thermal high point It is distilled to obtain liquefied coal coil and liquefied residue after mixing from 160 Partial Liquid Phase product of device, catalysis is carried out to liquefied coal coil and is added Hydrogen processing, provides the cycling solvent with stronger hydrogen supply capacity, so as to improve lique faction of coal conversion ratio and oil yield.
In Direct coal liquefaction device provided by the present invention, catalytic hydrogenation unit can include sequential communication surge tank 210 With catalytic hydrogenation reaction device 220, and the destilling tower oil phase outlet of surge tank 210 and vacuum distillation tower 180.It is urged by above-mentioned Change the catalytic hydrogenation treatment for the liquefied coal coil that hydrogenation unit can be realized to including second liquid phase product, so as to obtain coal liquefaction production Product and the coal liquefaction solvent with stronger hydrogen supply performance;Preferably, above-mentioned catalytic hydrogenation reaction device 220 for fixed bed reactors or Fluidized bed reactor;More preferably fluidized bed reactor, strong to adaptability to raw material, catalyst can be replaced online, ensure catalysis Agent bed is activity stabilized, so as to ensure that Xun Huan solvent property is stablized.
In Direct coal liquefaction device provided by the present invention, the exit of catalytic hydrogenation reaction device 220 can be cycled Solvent, i.e., Direct coal liquefaction device using the present invention directly can be hydrogenated with liquid phase during coal using solvent catalysis Liquid be fractionated in product, in addition to liquid fuel is as Xun Huan solvent.By being noted in the second liquefying reactor 150 Enter hydrogen and cycle hydrogen supply dissolvent, improve the hydrogen partial pressure and active amt in reaction process, to promotion be difficult to the coal converted and The conversion of pitch metallic substance is favourable, ensures that the reaction process in second reactor has higher hydrogen partial pressure and active amt, so as to carry High lique faction of coal conversion ratio and oil yield.
In preparation method provided by the present invention, liquefaction reaction uses the common reactor of those skilled in the art. In a preferred embodiment, the first liquefying reactor 130 and the second liquefying reactor 150 are independently selected from forced circulation Suspended-bed reactor, bubbling bed reactor, paste state bed reactor or the circulation flow reactor with guide shell are more preferably forced to follow Ring suspended-bed reactor, it is ensured that the flow rate of liquid in reactor reduces deposition of solids, and realization device long period is steady Fixed operating.
Above-mentioned introduction according to the present invention, those skilled in the art can select specific operating system, to coal is straight Connect liquefaction liquid fuel was prepared.Specific operating process can be as follows:
Become coal dust after coal is crushed, and after drying with Xun Huan solvent, catalyst for coal liquefaction in coal preparing tank 110 In be hybridly prepared into pump conveying coal slurry.Coal slurry is mixed after high-pressure coal pulp pump 101 boosts with hydrogen, into heating furnace 120, heat temperature raising.120 outlet temperature of heating furnace is controlled at 350 DEG C or more.
The first liquid that coal slurry after heated is exported with hydrogen into the first liquefying reactor 130, the first liquefying reactor 130 Change product and enter intermediate separator 140, temperature control is at 410~440 DEG C, and the residence time is less than 3 minutes, intermediate separator 140 The first liquid product (liquid phase material) of outlet is conveyed through coal liquefaction second reactor feed pump 102, and molten with hydrogen and Xun Huan Agent enters the second liquefying reactor 150 after mixing.In two liquefying reactors, controlling reaction temperature is 420~470 DEG C, pressure It is 800~1200L/Kg for 15~20MPa, hydrogen and coal slurry ratio, under the effect of the catalyst, liquefaction reaction generation occurs for coal dust Gas-phase product and liquid product mixture.Second liquefaction products of the second liquefying reactor 150 outlet divide into the first thermal high Oil-gas Separation is carried out from device 160, separation temperature is controlled at 400~420 DEG C;The of first high pressure hot separator, 160 top output It is separated after the first gas-phase product mixing that two gas-phase products are isolated with intermediate separator 140 after cooling into the first cold anticyclone Device 170;First cold high pressure separator 170 is controlled below 45 DEG C, and the discharge of top gas phase part returns to heating furnace as recycle hydrogen 120 entrances, are partly discharged, and the second liquid phase product section that 160 bottom of the first high pressure hot separator is isolated is recycled back to One liquefying reactor 130 and/or the second liquefying reactor 150;First cold high pressure separator, 170 bottom generate liquid product with Enter vacuum distillation tower 180 after another part liquid product mixing of first high pressure hot separator, 160 bottom.In vacuum distillation tower Separation of solid and liquid is carried out in 180, in order to ensure that coal liquefaction solvent fully recycles, while residue has good transportation performance, control The solid concentration being evaporated under reduced pressure in bottom of towe residue is 50~55%.
The liquefied coal coil of 180 output of vacuum distillation tower enters surge tank 210, after 103 boosting of hydrogenating materials pump, with hydrogen Into catalytic hydrogenation reaction device 220 after gas mixing preheating, catalytic hydrogenation reaction is carried out, realizes aromatic moiety hydrogenation saturation, simultaneously Generation work desulfurization, denitrogenation and deoxygenation.During catalytic hydrogenation reaction, control pressure be 8~20MPa, reaction temperature 320 ~390 DEG C, 0.5~2.0h of volume space velocity-1.The material that catalytic hydrogenation reaction device 220 exports output is separated into the second thermal high Device 230.The gas phase of second high pressure hot separator, 230 output is after supercooling into the second cold high pressure separator 240, temperature control System is below 45 DEG C.The discharge of second cold high pressure separator, 240 top gas phase part returns to hydrogenation catalyst reactant as recycle hydrogen System, is partly discharged;Second high pressure hot separator, 230 bottom liquid phases material flows into fractionating column 250 after decompression, is produced Product separate, and obtain liquid fuel and Xun Huan solvent, and the liquid fuel of formation includes naphtha and diesel oil.
The present invention is described in further detail below in conjunction with specific embodiment, these embodiments are it is not intended that limit this Invent scope claimed.
Embodiment 1
Coal direct liquefaction method provided in this embodiment carries out coal liquefaction experiment using DCL/Direct coal liquefaction long run test device, Device uses the suspended-bed reactor of two forced circulations, and intermediate separator is set between reactor, the second liquefying reactor Outlets products liquid-solid phase material parts after separation are recycled back to the first liquefying reactor entrance.Using refreshing eastern coal as test raw material coal, Feed coal is placed in coal slurry tank and mixed with catalyst, coal liquefaction Xun Huan solvent, obtains coal slurry, feed coal fundamental property is shown in Table 1, Above-mentioned coal direct liquefaction method comprises the following steps:
First, above-mentioned coal slurry liquefies with hydrogen into the first liquefying reactor (forced circulation suspended-bed reactor), first First liquefaction products of reactor outlet enter intermediate separator, and temperature is controlled at 430 DEG C, residence time 5min, centre point The first liquid product from device outlet convey through the second liquefying reactor feed pump, and with hydrogen and cycling after solvent mixes and entering the Two liquefying reactors (forced circulation suspended-bed reactor), in two liquefying reactors, controlling reaction temperature is 455 DEG C, instead Pressure 19.0MPa, hydrogen and coal ratio are answered as 1000L/Kg, and catalyst for coal liquefaction is artificial synthesized 863 catalyst, coal liquid Change catalyst loading is 1.0wt%, and auxiliary agent is sulphur, control n (S)/n (Fe)=2;The second of second liquefying reactor outlet Liquefaction products carry out Oil-gas Separation into the first high pressure hot separator, and separation temperature is controlled at 410 DEG C;First high pressure hot separator The first gas-phase product that the second gas-phase product and the intermediate separator of top output are isolated enters first after mixing after cooling Cold high pressure separator;First cold high pressure separator is controlled below 45 DEG C, and the discharge of top gas phase part is returned as recycle hydrogen to be added Hot stove entrance, is partly discharged, and the second liquid phase product section that the first high pressure hot separator bottom is isolated is recycled back to first Liquefying reactor 130, and part second liquid phase product and the first material quantity are than 0.3;What the first cold high pressure separator bottom generated Liquid product enters vacuum distillation tower after being mixed with another part liquid product of the first high pressure hot separator bottom, is steamed in decompression It evaporates and separation of solid and liquid is carried out in tower 180, it is 50% to control the solid concentration in vacuum distillation bottom of towe residue.
Then, the liquefied coal coil of output enters stabilized hydrogenation raw material surge tank in the middle part of vacuum distillation tower, by hydrogenating materials After pump boosting, enter catalytic hydrogenation reaction device (forced-circulation boiling bed hydroprocessing reactor) after preheating is mixed with hydrogen, urged Change hydrogenation reaction, realize aromatic moiety hydrogenation saturation, while desulfurization, denitrogenation and deoxygenation occurs;Catalytic hydrogenation reaction process In, control pressure 19MPa, reaction temperature is 380 DEG C, volume space velocity 1.0h-1, hydrogen-oil ratio 300, the outlet of catalytic hydrogenation reaction device The material of output enters the second high pressure hot separator;The gas phase of second high pressure hot separator output is cold into second after supercooling High-pressure separator, temperature are controlled below 45 DEG C;The discharge of second cold high pressure separator top gas phase part is returned as recycle hydrogen Hydrogenation catalyst reaction system is returned, is partly discharged;Second high pressure hot separator bottom liquid phases material flows into after decompression to be divided Tower is evaporated, carries out product separation, obtains the liquid fuel for including naphtha and diesel oil and Xun Huan solvent, and the temperature for cycling solvent is 220 DEG C of distillate.
Embodiment 2
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The inlet amount of part second liquid phase product and the first raw material is than 0.1.
Embodiment 3
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The inlet amount of part second liquid phase product and the first raw material is than 1.
Embodiment 4
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The inlet amount of part second liquid phase product and the second raw material is than 0.1.
Embodiment 5
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The inlet amount of part second liquid phase product and the second raw material is than 1.0.
Embodiment 6
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
Part second liquid phase product and the first raw material/inlet amount than 0.2, part second liquid phase product and the first raw material Inlet amount is than 0.3.
Embodiment 7
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The temperature of Coal liquefaction is 430 DEG C, and reaction pressure 15.0MPa, hydrogen and coal ratio are 750L/Kg.
Embodiment 8
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The temperature of Coal liquefaction is 460 DEG C, and reaction pressure 20.0MPa, hydrogen and coal ratio are 1200L/Kg.
Embodiment 9
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The additive amount of catalyst for coal liquefaction is 0.4wt%.
Embodiment 10
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The additive amount of catalyst for coal liquefaction is 2.0wt%.
Embodiment 11
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The pressure of solvent catalysis hydrotreating is 8MPa, and reaction temperature is 320 DEG C, volume space velocity 0.8h-1, hydrogen-oil ratio is 800。
Embodiment 12
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
The pressure of solvent catalysis hydrotreating is 19MPa, and reaction temperature is 390 DEG C, volume space velocity 2.0h-1, hydrogen-oil ratio For 800.
Embodiment 13
Coal direct liquefaction method provided in this embodiment and embodiment 1 difference lies in:
Liquefaction second reactor entrance is not injected into the solvent for cycling.
Comparative example 1
This comparative example and embodiment 1 difference lies in:
Coal liquefaction experiment is carried out using DCL/Direct coal liquefaction long run test device, which uses the suspension of two forced circulations Bed reactor, but intermediate separator is not provided between reactor, high score material does not cycle.
Comparative example 2
This comparative example and embodiment 1 difference lies in:
Coal liquefaction experiment is carried out using DCL/Direct coal liquefaction long run test device, which uses the suspension of two forced circulations Bed reactor, sets intermediate separator between reactor, second liquid phase product is not recycled to the first liquefying reactor and the second liquid Change reactor.
God east lique faction of coal reaction result is shown in Table 2 in above-described embodiment 1-13 and comparative example 1-2.
Table 1
Table 2
By table 2 as it can be seen that separation among setting under identical reaction conditions, between two tandem reactors of DCL/Direct coal liquefaction After device and high score material parts Xun Huan, gas yield has to be declined by a relatively large margin, is minimized 12.60% by 15.42%, is reduced by 3 More than percentage point, hydrogen consumption slightly decreases, and minimum 5.53% is reduced to by 5.79%;Simultaneously it is also found that the liquid of the eastern coal of god Change conversion ratio and increase to highest 92.21% by 88.89%, increase by 2 percentage points or more, while pitch yield also has apparent drop It is low, 7.21% is minimized by 10.49%, reduces by 3 percentage points or more;Distillation oil yield has and increases by a relatively large margin, by 53.79% increases to highest 59.92%, increases by 6 percentage points or more.
It is also known by table 2, intermediate separator is set between two tandem reactors of DCL/Direct coal liquefaction but high score material does not follow In the case of ring, gas yield is also decreased obviously, and 13.98% is minimized by 15.42%, reduces about 1.5 percentage points, hydrogen consumption Variation is little;Refreshing east lique faction of coal conversion ratio increases to highest 91.10% by 88.89%, increases by 1 percentage point or more, drips simultaneously Blue or green yield is also substantially reduced, and is minimized 8.77% by 10.49%, is reduced about 1.8 percentage points.
It is also known by table 2, sets intermediate point under identical reaction conditions, between two tandem reactors of DCL/Direct coal liquefaction From device, after high score material parts cycle, but the second liquefying reactor entrance is not injected into cycling solvent, and gas yield substantially rises, by 12.60% rises to 14.37%;Hydrogen consumes also more apparent increase, and 6.07% is increased to by 5.53%;The conversion ratio of coal is by 92.21% drop To 90.63%, 1.5 percentage points or more are reduced;Oil yield is down to 54.66% by 59.92%, reduce 5 percentage points with On, asphalitine yield increases to 9.98% by 7.21%, adds about 2.7 percentage points.
It can be seen from the above description that the above embodiments of the present invention realize following technique effect:
1st, added between first time liquefaction reaction and second of liquefaction reaction and oil gas point is carried out to the first liquefaction products From the step of, Coal liquefaction is divided into two relatively independent systems by a system, not only significantly reduces light oil Residence time avoids secondary cracking problem, reduces gas yield and hydrogen consumption, also helps and reduce gas in second of liquefaction reaction The delay of body, and then the residence time of more difficult transformation substance in the reaction is improved, the hydrogen partial pressure in reaction process is added, is had Beneficial to raising lique faction of coal conversion ratio and oil yield;
2nd, the first raw material and/or the second raw material further include the second liquid phase production that the second liquefaction products obtain after Oil-gas Separation Part second liquid phase product circulation is returned Coal liquefaction process by object, improve catalyst content in liquefaction reaction and compared with It is difficult to convert the residence time of coal and bitumen, and then improves lique faction of coal conversion ratio, ultimately increase coal liquefaction Oil yield improves resource utilization, enhances the competitiveness of direct coal liquefaction technology;
3rd, by injecting hydrogen and Xun Huan hydrogen supply dissolvent in second of liquefaction reaction, the hydrogen point in reaction process is improved Pressure and active amt, promotion are difficult to the coal converted and the oil for being further converted to small molecule of pitch metallic substance, are also beneficial to carry The conversion ratio and oil yield of high coal.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made any repaiies Change, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.

Claims (14)

1. a kind of coal direct liquefaction method, which is characterized in that comprise the following steps:
S1 makes the first raw material for including coal slurry and hydrogen carry out first time liquefaction reaction, obtains the first liquefaction products, and to described First liquefaction products carry out Oil-gas Separation, obtain the first liquid product;
S2 makes the second raw material for including first liquid product, hydrogen and solvent carry out second of liquefaction reaction, obtains second Liquefaction products, and Oil-gas Separation is carried out to second liquefaction products, obtain second liquid phase product;
S3, distills the part second liquid phase product and catalytic hydrogenation treatment, obtains Coal Liquefaction Products;And
S4 repeats above-mentioned steps S1 to S3, and first raw material and/or described during described repeat Two raw materials further include second liquid phase product described in remainder.
2. coal direct liquefaction method according to claim 1, which is characterized in that the remainder second liquid phase product with The inlet amount of first raw material is than 0.1~1, the inlet amount ratio of the remainder second liquid phase product and second raw material 0.1~1.
3. coal direct liquefaction method according to claim 1, which is characterized in that the first time liquefaction reaction and/or institute The pressure for stating second of liquefaction reaction is each independently 15~20MPa, and reaction temperature is each independently 440~460 DEG C, hydrogen The volume of gas and the weight ratio of coal slurry are each independently 800~1200L/Kg.
4. coal direct liquefaction method according to claim 1, which is characterized in that the coal slurry includes coal dust and coal liquefaction is urged Agent, preferably described catalyst for coal liquefaction include nanoscale hydrated ferric oxide, natural crystal, the compound of pure state iron and nanoscale Any one of ferrous sulfide is a variety of, and the more preferable catalyst for coal liquefaction is nanoscale hydrated ferric oxide;It is preferred that the coal The dosage of deliquescence accelerant accounts for 0.5~1.5wt% of the coal slurry.
5. coal direct liquefaction method according to claim 1, which is characterized in that in the step S1, to described first Liquefaction products carry out the temperature of Oil-gas Separation as 410~440 DEG C, and the time is less than 5min, and the preferably time is less than 3min.
6. coal direct liquefaction method according to claim 1, which is characterized in that in the step S2, to described second The temperature that liquefaction products carry out Oil-gas Separation is 380~430 DEG C.
7. coal direct liquefaction method according to claim 1, which is characterized in that in the step S3, the catalysis adds The pressure of hydrogen processing is 15~19MPa, and reaction temperature is 350~390 DEG C, and volume space velocity is 0.8~2.0h-1, hydrogen-oil ratio 300 ~800.
8. coal direct liquefaction method according to claim 1, which is characterized in that in the step S3, urged using hydrogenation Agent carries out the second liquid phase product after distillation catalytic hydrogenation treatment, and the hydrogenation catalyst is loaded catalyst, Preferred vector is aluminium oxide, and the active metal component of the loaded catalyst is any one of group vib or VIII group or more Kind, the metal component of more preferable group vib is Mo and W, and the metal component of VIII group is Ni and Co.
9. coal direct liquefaction method according to claim 4, which is characterized in that the part second liquid phase product into Xun Huan solvent is also obtained in the step of row catalytic hydrogenation treatment, during described repeat, first raw material includes Part the cycling solvent, the solvent in second raw material is cycles solvent described in another part, preferably described cycling Solvent is more than 220 DEG C of distillate for temperature, and density is 0.92~0.99g/cm3
10. coal direct liquefaction method according to claim 1, which is characterized in that carried out to first liquefaction products The first gas-phase product is obtained in the step of Oil-gas Separation, and is obtained in the step of carrying out Oil-gas Separation to second liquefaction products To the second gas-phase product, the step S3 further includes procedure below at this time:
Oil-gas Separation is carried out to the mixture of first gas-phase product and second gas-phase product, obtains the production of the 3rd liquid phase Object;
3rd liquid product is distilled and catalytic hydrogenation treatment, preferably to the 3rd liquid product and described second The mixture of liquid product carries out the distillation and the catalytic hydrogenation treatment.
11. a kind of Direct coal liquefaction device, which is characterized in that the Direct coal liquefaction device includes:
First liquefying reactor (130) has first circulation material inlet and the first product exit;
Intermediate separator (140) has the first product inlet and the first liquid-phase outlet, first product inlet and described first Product exit connects;
Second liquefying reactor (150) has the second feed(raw material)inlet, second circulation material inlet and the second product exit, described Second feed(raw material)inlet is connected with first liquid-phase outlet;
First high pressure hot separator (160) there is the second product inlet and second liquid phase to export, second product inlet and institute The connection of the second product exit is stated, the second liquid phase outlet enters with the first circulation material inlet and the second circulation material Mouth connection;
Vacuum distillation tower (180) has destilling tower entrance, the outlet of destilling tower oil phase and destilling tower solid-phase outlet, the destilling tower Entrance and the second liquid phase outlet;And
Solvent catalysis hydrogenation unit, with the destilling tower oil phase outlet.
12. Direct coal liquefaction device according to claim 11, which is characterized in that the intermediate separator (140) also has There is the first gaseous phase outlet, first high pressure hot separator (160) also has the second gaseous phase outlet, the Direct coal liquefaction device The first cold high pressure separator (170) is further included, and first cold high pressure separator (170) goes out respectively with first gas phase Mouth, second gaseous phase outlet are connected with the vacuum distillation tower entrance.
13. Direct coal liquefaction device according to claim 11, which is characterized in that first liquefying reactor (130) It is anti-independently selected from forced circulation suspended-bed reactor, bubbling bed reactor, slurry bed system with second liquefying reactor (150) Device and the circulation flow reactor with guide shell are answered, is preferably forced circulation suspended-bed reactor.
14. Direct coal liquefaction device according to claim 11, which is characterized in that the solvent catalysis hydrogenation unit includes The surge tank (210) of sequential communication and catalytic hydrogenation reaction device (220), and the surge tank (210) and the vacuum distillation tower (180) connect, preferably described catalytic hydrogenation reaction device (220) is fixed bed reactors or fluidized bed reactor, is more preferably boiled Rise a reactor.
CN201711203668.6A 2017-11-24 2017-11-24 Direct coal liquefaction method and direct coal liquefaction device Active CN108048121B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711203668.6A CN108048121B (en) 2017-11-24 2017-11-24 Direct coal liquefaction method and direct coal liquefaction device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711203668.6A CN108048121B (en) 2017-11-24 2017-11-24 Direct coal liquefaction method and direct coal liquefaction device

Publications (2)

Publication Number Publication Date
CN108048121A true CN108048121A (en) 2018-05-18
CN108048121B CN108048121B (en) 2020-12-08

Family

ID=62120618

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711203668.6A Active CN108048121B (en) 2017-11-24 2017-11-24 Direct coal liquefaction method and direct coal liquefaction device

Country Status (1)

Country Link
CN (1) CN108048121B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108641741A (en) * 2018-05-23 2018-10-12 华东理工大学 A kind of liquefied process of coal multistage composite catalytic hydrogenation
CN108998068A (en) * 2018-08-22 2018-12-14 国家能源投资集团有限责任公司 DCL/Direct coal liquefaction system and coal direct liquefaction method
CN112552964A (en) * 2019-09-10 2021-03-26 南京延长反应技术研究院有限公司 Micro-interface-based system and process for strengthening coal indirect liquefaction

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587351A (en) * 2004-07-30 2005-03-02 神华集团有限责任公司 Method for directly liquefying coal
CN101987962A (en) * 2010-11-12 2011-03-23 煤炭科学研究总院 Method for liquefying high-oxygen content coal by adopting direct hydrogenation
CN102010741A (en) * 2010-11-26 2011-04-13 煤炭科学研究总院 Method for directly liquefying coals with function of maximizing utilization of liquefied residues
CN102115674A (en) * 2009-12-30 2011-07-06 中国石油化工股份有限公司 Coal liquefaction and petroleum refining combined method
CN102191072A (en) * 2010-03-18 2011-09-21 Ifp新能源公司 Coal conversion process and products, comprising two direct ebullated bed liquefaction stages and a fixed bed hydrocracking stage
CN107163974A (en) * 2017-06-21 2017-09-15 华东理工大学 A kind of multistage supplies the direct coal liquefaction process method of hydrogen supply dissolvent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587351A (en) * 2004-07-30 2005-03-02 神华集团有限责任公司 Method for directly liquefying coal
CN102115674A (en) * 2009-12-30 2011-07-06 中国石油化工股份有限公司 Coal liquefaction and petroleum refining combined method
CN102191072A (en) * 2010-03-18 2011-09-21 Ifp新能源公司 Coal conversion process and products, comprising two direct ebullated bed liquefaction stages and a fixed bed hydrocracking stage
CN101987962A (en) * 2010-11-12 2011-03-23 煤炭科学研究总院 Method for liquefying high-oxygen content coal by adopting direct hydrogenation
CN102010741A (en) * 2010-11-26 2011-04-13 煤炭科学研究总院 Method for directly liquefying coals with function of maximizing utilization of liquefied residues
CN107163974A (en) * 2017-06-21 2017-09-15 华东理工大学 A kind of multistage supplies the direct coal liquefaction process method of hydrogen supply dissolvent

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108641741A (en) * 2018-05-23 2018-10-12 华东理工大学 A kind of liquefied process of coal multistage composite catalytic hydrogenation
CN108641741B (en) * 2018-05-23 2021-03-26 华东理工大学 Coal multistage composite catalytic hydrogenation liquefaction process method
CN108998068A (en) * 2018-08-22 2018-12-14 国家能源投资集团有限责任公司 DCL/Direct coal liquefaction system and coal direct liquefaction method
CN112552964A (en) * 2019-09-10 2021-03-26 南京延长反应技术研究院有限公司 Micro-interface-based system and process for strengthening coal indirect liquefaction

Also Published As

Publication number Publication date
CN108048121B (en) 2020-12-08

Similar Documents

Publication Publication Date Title
CN101993721B (en) Method of liquid phase circulation hydrotreatment and reactive system
CN110484296A (en) A kind of adverse current type multiphase flow hydrocracking heavy oil technique
CN104611019B (en) A kind of low energy consumption method for hydrogen cracking producing high-quality jet fuel
CN104388117A (en) Method for producing high-quality fuel oil by heavy oil hydrocracking
CN108048121A (en) Coal direct liquefaction method and Direct coal liquefaction device
CN107057742A (en) Coal liquefaction method and device
CN102120934A (en) Circulating liquid phase hydrogenation method
CN104611025B (en) A kind of low energy consumption method for hydrogen cracking producing high-quality industrial chemicals
CN103627427B (en) Two-stage hydrogenation system, and hydrogenation method
CN104388116A (en) High-efficiency heavy inferior oil conversion process
CN108659882A (en) A kind of Heavy oil hydrogenation method and its hydrogenation system
CN108998068A (en) DCL/Direct coal liquefaction system and coal direct liquefaction method
CN104531197B (en) A kind of preparation method of liquid fuel
CN107815329B (en) A kind of method of heavy oil combined hydrogenation
CN105602601A (en) Coal-to-oil catalytic extraction technology and special device thereof
CN103865575B (en) A kind of method of high nitrogen catalytic cracking diesel oil liquid phase circulation hydro-upgrading
CN104650970B (en) A kind of hydrocracking method reducing light fraction product sulfur content
CN105733669A (en) Oil product hydrogenation method
CN107629816B (en) A kind of Heavy oil hydrogenation method
CN108456550A (en) A kind of outer circulation type reaction unit and kerosene are total to smelting method
CN105754649B (en) A kind of method for improving hydrocracking unit safety in operation
CN101724441B (en) Combined technical method for modifying heavy oil
CN112877090A (en) Coal direct liquefaction circulating solvent and preparation method and system thereof
CN102465016B (en) Combined hydrogenation process
CN101875856A (en) Wax oil hydrogenated treatment and catalytic cracking combined method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant