CN104845652B - The processing method of coal directly-liquefied residue - Google Patents
The processing method of coal directly-liquefied residue Download PDFInfo
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- CN104845652B CN104845652B CN201510317246.6A CN201510317246A CN104845652B CN 104845652 B CN104845652 B CN 104845652B CN 201510317246 A CN201510317246 A CN 201510317246A CN 104845652 B CN104845652 B CN 104845652B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
Abstract
The present invention provides a kind of processing methods of coal directly-liquefied residue.This method includes：Coal directly-liquefied residue is extracted using extractant, obtains extraction mixture；Level-one separation of solid and liquid is carried out to extraction mixture, obtains level-one clear liquid and primary concentration phase；All or part of level-one clear liquid is subjected to two level separation of solid and liquid, obtains two level clear liquid and secondary concentration phase；All or part of two level clear liquid is subjected to three-level separation of solid and liquid, obtains three-level clear liquid and three-level concentration phase；Two level separation of solid and liquid is carried out to the level-one clear liquid of part, clear liquid solvent recovery processing is carried out to remaining level-one clear liquid, obtains level-one pitch；Three-level separation of solid and liquid is carried out to the two level clear liquid of part, clear liquid solvent recovery processing is carried out to remaining two level clear liquid, obtains two level pitch；And clear liquid solvent recovery processing is carried out to whole three-level clear liquids, obtain three-level pitch.This method can obtain three kinds of asphaltic products, be conducive to improve the add on yield value of pitch in coal liquefaction residue.
Description
Technical field
The present invention relates to coal chemical technology, in particular to a kind of processing method of coal directly-liquefied residue.
Background technology
Coal directly-liquefied residue is the non-targeted product of DCL/Direct coal liquefaction process, accounts for about the 30% of coal feeding amount.It is a kind of
The substance of high ash, high-sulfur and high heating value, mainly distillates liquefaction oil (n-hexane soluble matter), pitch (the insoluble tetrahydrochysene of n-hexane by non-
Furans soluble matter), unconverted coal and inanimate matter composition.It is non-to distillate liquefaction oil (heavy coal liquids) and pitch accounts for about DCL/Direct coal liquefaction
The 50% of residue is mainly made of polycyclic condensed aromatics, with aromaticity height, easily carbon content height, polymerization or crosslinked spy
Point.Different with the characteristic of asphalt and coal tar asphalt, the bitumen in coal directly-liquefied residue is very suitable for
It is a kind of valuable and unique carbon resource as the raw material for preparing carbon material；Unconverted coal refers to not dissolve in tetrahydrochysene in residue
The organic matter of furans accounts for about the 30% of residue total amount, has higher calorific value；Inanimate matter is mainly by the minerals in coal and outside
The catalyst composition added, accounts for about the 20% of residue total amount.
How to be efficiently rationally very important subject in coal liquefaction craft using coal directly-liquefied residue.Now, state
The method of interior large-scale application coal directly-liquefied residue is that coal directly-liquefied residue and coal are deployed into water-coal-slurry, as gasification furnace
Raw material prepares synthesis gas and hydrogen, this has found outlet for coal directly-liquefied residue large-scale application, realizes residue as resources
It utilizes.However high added value is not implemented in coal directly-liquefied residue, tetrahydrofuran soluble matter (bitumen) particularly therein
Utilization, so as to which maximization is not implemented in the economic benefit for causing DCL/Direct coal liquefaction industry.It will be solvable in coal directly-liquefied residue
Part and insoluble portion separate, and then above-mentioned two parts are reasonably developed and used respectively, can generate larger economy
Benefit and social benefit.
The Japan Patent of Publication No. JPS5984977A provides a kind of method for extracting organic matter in liquefied residue, will
It extracts obtained organic matter (including heavy coal liquids and asphaltene) and all carries out secondary hydrocracking, obtain light naphtha,
So as to improve the yield of overall liquefaction oil.However, as the presence of bitumen, this method is easy to generate secondary plus hydrogen and urges
The problem of agent inactivates due to carbon deposit.
The Japan Patent of Publication No. JPH0130412A provides one kind and heavy liquid is isolated from coal directly-liquefied residue
The method of carburetion and bitumen.The heavy coal liquids of separation are carried out secondary hydrocracking and obtain lightweight liquefaction by this method
Oil, while bitumen is entered into coal liquefaction unit and carries out re-liquefied reaction.There are probelem in two aspects for this method：One side
Face, since the fraction of heavy coal liquids is than heavier, arene content is higher, does not require nothing more than carry out deep hydrogenation, leads to hydrogen consumption
Increase, and be easy to cause hydrogenation catalyst and inactivated due to coking；On the other hand, liquid again is carried out to the bitumen isolated
During change, re-liquefied effect is simultaneously bad, but also can cause the ill effects such as deposition, coking in liquefying reactor, therefore should
Method can not realize the reasonable efficient utilization of bitumen.
Grant number is that the Chinese patent of CN101885976 discloses one kind extraction pitch class object from coal directly-liquefied residue
The method of matter and liquefaction heavy oil, using distillate self-produced during DCL/Direct coal liquefaction as extractant, by bitumen
It is come out, then the method using destructive distillation with liquefaction mink cell focus together extraction and separation, bitumen and liquefaction heavy oil is opened, obtained
To mesophase pitch, liquefaction mink cell focus moderately plus after hydrogen returns to coal liquefaction unit.Liquefaction mink cell focus is mainly evaporating more than 450 DEG C
It is grouped as, it is stronger with bitumen binding force, when being detached using the method for high-temperature retorting, on the one hand lead to the mink cell focus that liquefies
Cracking, on the other hand leads to bituminous material coking, and is difficult to use as the cycle solvent of coal liquefaction.
Grant number be CN101962560A and CN101962561A patent individually disclose it is a kind of using two-stage extraction from
The method that heavy coal liquids and bitumen are extracted in coal directly-liquefied residue, this method are produced with DCL/Direct coal liquefaction process itself
The oil product of two raw different fractions sections is extractant, carries out two-stage sequence to liquefied residue respectively and extracts, obtains heavy liquid
Carburetion and bitumen.But this method is using two-stage extraction and two-stage separation of solid and liquid, thus technological process is complicated, while raw material
Extractant source is single and higher price, and product yield is relatively low, and cost is higher, and obtained bitumen softening point
Height, volatile matter is low, and product development applicability is not strong.
Presence in view of the above problems, it is necessary to a kind of processing method of coal directly-liquefied residue is developed, to improve coal
The add on yield value of bitumen in direct liquefaction residue.
Invention content
It is a primary object of the present invention to provide a kind of processing method of coal directly-liquefied residue, to solve in the prior art
The problem of add on yield value of bitumen is relatively low in coal directly-liquefied residue realizes the efficient comprehensive profit of coal liquefaction residue
With.
To achieve these goals, one aspect of the invention provides a kind of processing method of coal directly-liquefied residue, should
Method includes：Coal directly-liquefied residue is extracted using extractant, obtains extraction mixture；Extraction mixture is carried out
Level-one separation of solid and liquid obtains level-one clear liquid and primary concentration phase；All or part of level-one clear liquid is subjected to two level separation of solid and liquid,
Obtain two level clear liquid and secondary concentration phase；All or part of two level clear liquid is subjected to three-level separation of solid and liquid, obtains three-level clear liquid
Phase is concentrated with three-level；Two level separation of solid and liquid is carried out to the level-one clear liquid of part, carrying out clear liquid solvent to remaining level-one clear liquid returns
Receipts processing, obtains level-one pitch；Three-level separation of solid and liquid is carried out to the two level clear liquid of part, clear liquid is carried out to remaining two level clear liquid
Solvent recovery processing, obtains two level pitch；And clear liquid solvent recovery processing is carried out to whole three-level clear liquids, obtain three-level drip
It is green.
Further, extractant is selected from tetrahydrofuran, furfural, N-Methyl pyrrolidone, quinoline, toluene, the direct liquid of coal
Change one or more in the group of distillate or dead oil composition.
Further, by coal directly-liquefied residue and extractant with weight ratio 1:1~8 mixing, in N2Or inert gas
Protection, 0.01~1MPa, extraction process is carried out under conditions of 30~200 DEG C；Wherein, extraction time is 5~60min, and stirring is fast
Rate is 25~150r/min.
Further, the method for level-one separation of solid and liquid, two level separation of solid and liquid and three-level separation of solid and liquid is separately selected
Inherent filtration, cyclonic separation method, centrifugal separation or sedimentation separation method.
Further, when using can when being separated by filtration method of serialization, separation temperature is 30~200 DEG C, pressure for 0.1~
1.0MPa；When using cyclonic separation method, separation temperature is 30~200 DEG C, and pressure is 0.2~0.6MPa；When using centrifugation point
During from method, separation temperature is 30~200 DEG C, and pressure is 0.01~0.05MPa；When using sedimentation separation method, separation temperature is
30~200 DEG C, pressure is 0.01~0.1MPa.
Further, the solid content of primary concentration phase is 50~80wt%, the solid content of secondary concentration phase for 15~
50wt%, the solid content of three-level concentration phase is 10~45wt%.
Further, the method for clear liquid solvent recovery is air-distillation, vacuum distillation or evaporation.
Further, the concentration of primary concentration phase, secondary concentration and three-level is mutually subjected to solvent recovery processing, obtains solid slag；
Preferably, solid content >=95wt% in solid slag.
Further, the concentration of primary concentration phase, secondary concentration and three-level is mutually subjected to the method for solvent recovery processing to subtract
Press distillation, air-distillation, vacuum drying, microwave drying or stripping.
Further, using weight ratio as 1：0~5, solid slag and coal are configured to the water-coal-slurry that solid content is 50~80wt%,
Then water-coal-slurry is gasified and is burnt；Preferably, level-one pitch can be used for road asphalt and waterproof roll field；It is preferred that
Ground, two level pitch can be used as impregnating agent and binding agent to use；Preferably, three-level pitch can be used for preparing needle coke, Carbon fiber
Dimension, mesocarbon microspheres or super-activated carbon.
It applies the technical scheme of the present invention, what coal directly-liquefied residue included non-distillates liquefaction oil (n-hexane soluble fraction)
It is very much like with the property of bitumen (n-hexane insoluble tetrahydrofuran soluble fraction), it is difficult to the two is completely separable, and
Separation costs are higher, are not suitable for carrying out industrial applications, and the comprehensive performance of obtained pitch is poor.And it is provided by the invention on
It states in processing method, continuous extraction separation has been carried out to coal directly-liquefied residue, liquefaction oil and bitumen are being distillated by non-
After extracting together, continuous solid-liquid separation treatment three times is carried out to extraction mixture respectively, level-one pitch, two can be obtained
Grade pitch and three-level pitch.These three asphaltic products can be applied in different application scenarios when with different physical property.This
It can either avoid because proposing non-of high cost, the insufficient problem of separation for distillating liquefaction oil and bitumen and bringing respectively, moreover it is possible to
It is enough that specific asphaltic products are prepared according to application demand.So as to significantly improve coal liquid under the premise of production cost is reduced
Change the pitch add on yield value in residue, coal liquefaction residue is made more to be integrated, more fully recycled.In addition, the application
Coal directly-liquefied residue is handled using continuous extraction and separation mode, also helps and realizes that large-scale industrial production should
With.
Description of the drawings
The accompanying drawings which form a part of this application are used to provide 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 the process flow diagram of the processing method of coal directly-liquefied residue provided by the invention.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the application 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.
As background technology part is described, using prior art, there are bitumens in coal directly-liquefied residue
The problem of add on yield value is not high.In order to solve this problem, the present invention provides a kind of processing sides of coal directly-liquefied residue
Method, as shown in Figure 1, the processing method includes：Coal directly-liquefied residue is extracted using extractant, obtains extraction mixing
Object；Level-one separation of solid and liquid is carried out to extraction mixture, obtains level-one clear liquid and primary concentration phase；All or part of level-one is clear
Liquid carries out two level separation of solid and liquid, obtains two level clear liquid and secondary concentration phase；All or part of two level clear liquid progress three-level is consolidated
Liquid detaches, and obtains three-level clear liquid and three-level concentration phase；Two level separation of solid and liquid is carried out to the level-one clear liquid of part, it is clear to remaining level-one
Liquid carries out clear liquid solvent recovery processing, obtains level-one pitch；Three-level separation of solid and liquid is carried out to the two level clear liquid of part, to remaining
Two level clear liquid carries out clear liquid solvent recovery processing, obtains two level pitch；And clear liquid solvent is carried out to whole three-level clear liquids and is returned
Receipts processing, obtains three-level pitch.
Level-one clear liquid can be handled according to demand there are many mode in the present invention：Part or all of level-one clear liquid carries out clear liquid
Solvent recovery processing, the level-one clear liquid of remainder carry out two level solid-liquid separation treatment, can also whole level-one clear liquids progress two
Grade separation of solid and liquid；Similarly, two level clear liquid can be handled there are many mode：It is molten that part or all of two level clear liquid carries out clear liquid
Agent is recycled, and the two level clear liquid of remainder carries out three-level solid-liquid separation treatment, can also all second-order clear liquid progress three-level
Separation of solid and liquid.According to the demand of level-one, two level and three-level pitch, the processing allocation proportion of level-one clear liquid, two level clear liquid is adjusted.
What coal directly-liquefied residue included non-distillate liquefaction oil (n-hexane soluble fraction) (n-hexane is not with bitumen
Molten tetrahydrofuran soluble fraction) property it is very much like, it is difficult to it is the two is completely separable, and separation costs are higher, be not suitable for into
Row industrial applications, and the comprehensive performance of obtained pitch is poor.And in above-mentioned processing method provided by the invention, it is direct to coal
Liquefied residue has carried out continuous extraction separation, is distillated after liquefaction oil and bitumen extract together by non-, right respectively
Extraction mixture has carried out continuous solid-liquid separation treatment three times, can obtain level-one pitch, two level pitch and three-level pitch.This three
Kind of asphaltic products can be applied in different application scenarios when with different physical property.This can either be avoided non-because proposing respectively
Distillate of high cost, the insufficient problem of separation that liquefaction oil and bitumen are brought, additionally it is possible to which spy is prepared according to application demand
Fixed asphaltic products.So as to the pitch add on yield in coal liquefaction residue is significantly improved under the premise of reducing production cost
Value, makes coal liquefaction residue more be integrated, more fully recycled.In addition, the application uses continuous extraction and separation mode
Coal directly-liquefied residue is handled, also helps and realizes large-scale industrial production application.
Specifically, be 120 DEG C~170 DEG C by the softening point of level-one pitch that above-mentioned processing method obtains, volatile matter
Content is 30~50wt%, and content of ashes is 0.5~5wt%；The softening point of two level pitch is 100~160 DEG C, volatile matter content
For 40~60wt%, content of ashes is 0.2~0.5wt%；The softening point of three-level pitch is 85~150 DEG C, and volatile matter content is
42~65wt%, content of ashes<0.1wt%.It can be seen that in separation of solid and liquid process, pitch that different phase is isolated
Property is different, this is conducive to user and selects rational occupation mode according to the heterogeneity of pitch, so as to improve the direct liquid of coal
Change the add on yield of bitumen in residue, and then improve the economic benefit of entire technique.
In addition, the application carries out using multistage separation of solid and liquid, multiple clear liquid solvent recovery and mutually solvent time to concentrating
It brings drill to an end work, this can realize the recycling of extractant in coal directly-liquefied residue separation process, improve the yield of product；Together
Shi Shangshu pitches, which need not carry out further deep processing, to come into operation, thus the processing method that the application provides has operation
It is simple for process, the advantages that cost is relatively low.
In above-mentioned processing method, organic solvent commonly used in the art may be used in extractant.It is preferably carried out in one kind
In mode, in step S1, extractant includes but not limited to tetrahydrofuran, furfural, N-Methyl pyrrolidone, quinoline, toluene, coal
It is one or more in the group of direct liquefaction distillate or dead oil composition.Term " DCL/Direct coal liquefaction distillate " can be with
It is distillate of the coal direct liquefaction oil in any fraction section, while term " dead oil " can be that coal tar is evaporated any
The distillate of segmentation.Be conducive to improve the solubility of the bitumen in coal directly-liquefied residue using above-mentioned solvent, so as to
Improve the yield of pitch, the final add on yield for improving bitumen in coal directly-liquefied residue.
In above-mentioned processing method, common operating condition may be used in extraction process.It is preferably carried out in mode in one kind,
By coal directly-liquefied residue and extractant with weight ratio 1:1~8 mixing, in N2Or inert gas shielding, 0.01~1MPa and
It is extracted under conditions of 30~200 DEG C, extraction time is 5~60min, and stir speed (S.S.) is 25~150r/min.Using above-mentioned
Extraction conditions is conducive to further improve the yield of extraction mixture, and then further improves pitch class in coal directly-liquefied residue
The add on yield of substance.Lower-cost mesolow water vapour may be used in above-mentioned extraction process to be kept the temperature.
In above-mentioned processing method, those skilled in the art can select the method for separation of solid and liquid.It is preferably carried out in one kind
In mode, the method for level-one separation of solid and liquid, two level separation of solid and liquid and three-level separation of solid and liquid is separately selected from filtration method, rotation
Flow separation method, centrifugal separation or sedimentation separation method.Using the method for above-mentioned separation of solid and liquid be conducive to improve level-one separation of solid and liquid,
The separative efficiency of two level separation of solid and liquid and three-level separation of solid and liquid process.
In above-mentioned processing method, those skilled in the art can select the temperature and pressure of separation of solid and liquid.A kind of preferred
In ground embodiment, when using filtration method, separation temperature is 30~200 DEG C, and separating pressure is 0.1~1.0MPa；Work as use
During cyclonic separation method, separation temperature is 30~200 DEG C, and inlet pressure is 0.2~0.6MPa；When using centrifugal separation, point
It it is 30~200 DEG C from temperature, separating pressure is 0.01~0.05MPa；When using sedimentation separation method, the temperature of separation for 30~
200 DEG C, pressure is 0.01~0.1MPa.It is detached using above-mentioned separation temperature, advantageously reduces the viscosity of extraction mixed liquor,
So as to further improve separative efficiency.Simultaneously according to different solid-liquid isolation methods, be conducive to further carry using different pressure
High score from efficiency.
In above-mentioned processing method, those skilled in the art can select respectively primary concentration phase, secondary concentration phase and
The content of solid content and solvent in three-level concentration phase.It is preferably carried out in mode in one kind, the solid content of primary concentration phase is 50
~80wt%, the solid content of secondary concentration phase is 15~50wt%, and the solid content of three-level concentration phase is 10~45wt%.By level-one
The content of solid content and solvent, which is each defined in above range, in concentration phase, secondary concentration phase and three-level concentration phase is conducive to
Solid-liquid separation efficiency is improved, while shortens the solvent recovery time.
In above-mentioned processing method, those skilled in the art can select to carry out the clear liquid that separation of solid and liquid process obtains molten
The method of agent recycling.Be preferably carried out in mode in one kind, the method for clear liquid solvent recovery include air-distillation, vacuum distillation or
Evaporation.Be conducive to improve the organic efficiency of solvent using the above method, so as to be conducive to further improve the utilization ratio of solvent,
Reduce the cost of coal directly-liquefied residue processing method.
In a preferred embodiment, the concentration of primary concentration phase, secondary concentration and three-level is mutually subjected to solvent recovery
Processing, obtains solid slag.This is conducive to obtain those skilled in the art is rationally applied according to actual needs.Preferably, solid slag
In solid content >=95wt%.Solid content in solid slag is limited to the recycling for, being conducive to improve solvent within the above range
Rate.
In above-mentioned processing method, those skilled in the art can select mutually to carry out the concentration that separation of solid and liquid process obtains
The method of solvent recovery.In a preferred embodiment, the concentration of primary concentration phase, secondary concentration and three-level is mutually carried out molten
The method of agent recovery processing includes but not limited to vacuum distillation, air-distillation, vacuum drying, microwave drying or stripping.Using upper
The method of stating is conducive to improve the organic efficiency of solvent, and so as to be conducive to further improve the utilization ratio of solvent, it is direct to reduce coal
The cost of liquefied residue processing method.
In above-mentioned processing method, solid slag may be used using method by the way of the routine of this field.A kind of preferred
In ground embodiment, using weight ratio as 1：0~5, solid slag and coal are configured to the water-coal-slurry that solid content is 50~80wt%, then
Above-mentioned water-coal-slurry is gasified and burnt.Solid slag is configured to the laggard promoting the circulation of qi of water-coal-slurry and burning with coal with aforementioned proportion has
Conducive to the utilization ratio for improving solid slag.Preferably, by level-one asphalt applications in road asphalt and waterproof roll field.Preferably,
Two level coal liquefaction pitch is used as impregnating agent and binding agent；Preferably, by three-level pitch be used to prepare needle coke, Carbon fibe, in
Between phase carbon microspheres or super-activated carbon.The output of above-mentioned three kinds of variety classes pitches is conducive to further improve DCL/Direct coal liquefaction
The add on yield of bitumen in residue, and then improve the economic benefit of entire technique.
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 range claimed.
Embodiment 1
Coal directly-liquefied residue (300kg/h) with tetrahydrofuran (300kg/h) in the stirred tank of 50L is mixed, is stirred
Kettle is protected using nitrogen, is 0.02MPa in pressure, under 60 DEG C of constant temperature, carries out extraction process, obtains extraction mixture.
By above-mentioned extraction mixture enter primary cyclone carry out level-one separation of solid and liquid, eddy flow temperature be 60 DEG C, one
The inlet pressure of grade cyclone separator is 0.2MPa；After level-one separation of solid and liquid, the flow of primary concentration phase is 185kg/h,
Level-one clear liquid total flow is 415kg/h, and the level-one stillness of night of wherein 265kg/h is sent into cross-flow filter progress two level in two level and is consolidated
Liquid detaches.
In two level separation of solid and liquid process, separation temperature is 60 DEG C, and the inlet pressure of cross-flow filter is 0.2MPa in two level,
The filter core aperture size of filter is 2 μm, and after secondary filtration, the flow of secondary concentration phase is 21kg/h, two level clear liquid stream
It measures as 244kg/h, the two level clear liquid of 120kg/h therein is sent into cross-flow filter in three-level carries out three-level separation of solid and liquid.
In three-level separation of solid and liquid process, separation temperature is 60 DEG C, and the inlet pressure of cross-flow filter is in three-level
0.18MPa, the filter core aperture size of filter is 50nm, and after three-stage filtration, the flow of three-level concentration phase is 12kg/h, three
Grade clear liquid flow is 108kg/h.
The three-level clear liquid of the level-one clear liquid of remaining 150kg/h, the two level clear liquid of 124kg/h and 108kg/h is sent respectively
Enter vacuum distillation tower, recovered overhead extractant (tetrahydrofuran) is recycled, and bottom of towe is collected into respectively：Softening point is
120 DEG C, the level-one pitch (56.kg/h) that volatile matter content 50wt%, ash content are 4.8wt%, softening point is 100 DEG C, volatilization
Point two level pitch (45kg/h) that content is 60wt%, ash content is 0.28wt% and softening point are 85 DEG C, and volatile matter content is
65wt%, the three-level pitch (40.kg/h) that ash content is 0.05wt%.Wherein, level-one pitch can as the modifying agent of road asphalt,
Two level pitch can be as the raw material of needle coke as the raw material of dipping agent bitumen, three-level pitch.
Primary concentration is mutually sent into vacuum drying unit, and recycling obtains the extractant of 35.5kg/h, can be recycled, obtains
The extract remainder (solid slag) of 149.5kg/h；Secondary concentration phase and three-level concentration mutually enter atmospheric distillation tower together, and recycling obtains
The extractant of 24kg/h, can be recycled, and extract remainder (solid slag) is 9kg/h.Extract remainder (solid slag) is with coal according to 1:5 quality
Than being configured to the water-coal-slurry that solid concentration is 50wt%, it is sent into gasification furnace and gasifies.
In the present embodiment the total recovery of level-one pitch, two level pitch and three-level pitch be 47.16wt%, the yield of solid slag
For 52.84wt%.
Embodiment 2
Coal directly-liquefied residue (250kg/h) is mixed with quinoline (500kg/h) in the stirred tank of 120L, stirred tank is adopted
It is protected with nitrogen, is 0.01MPa in pressure, under 100 DEG C of constant temperature, carry out extraction process, obtain extraction mixture.
By above-mentioned extraction mixture be passed through first-stage centrifugal seperator carry out level-one separation of solid and liquid, centrifuging temperature be 100 DEG C, one
The inlet pressure of grade centrifugal separator is 0.05MPa, centrifuge speed 3000r/min, after level-one separation of solid and liquid, level-one
The flow for concentrating phase is 150kg/h, and level-one clear liquid total flow is 600kg/h, and the level-one clear liquid of wherein 400kg/h is sent into two level
Centrifugal separator carries out two level separation of solid and liquid.
In two level separation of solid and liquid process, separation temperature is 100 DEG C, and the inlet pressure of two-stage centrifugal seperator is 0.04MPa,
Centrifuge speed is 7000r/min, and after two level separation of solid and liquid, the flow of secondary concentration phase is 28kg/h, two level clear liquid stream
It measures as 372kg/h, the two level clear liquid of 200kg/h therein is sent into cross-flow filter in three-level carries out three-level separation of solid and liquid.
In three-level separation of solid and liquid process, separation temperature is 100 DEG C, and the inlet pressure of cross-flow filter is in three-level
0.3MPa, the filter core aperture size of filter is 20nm, and after three-stage filtration, the flow of three-level concentration phase is 20kg/h, three
Grade clear liquid flow is 180kg/h.
The three-level clear liquid of the level-one clear liquid of remaining 200kg/h, the two level clear liquid of 172kg/h and 120kg/h is sent respectively
Enter vacuum distillation tower, recovered overhead extractant (quinoline) recycles, and bottom of towe is collected into respectively：Softening point is 151 DEG C, volatilization
Point level-one pitch (46kg/h) that content is 42.wt%, ash content is 4.2wt%, softening point are 137 DEG C, and volatile matter content is
48wt%, the two level pitch (39.kg/h) that ash content is 0.35wt% and softening point are 109 DEG C, volatile matter content 55wt%,
Ash content is the three-level pitch (34.kg/h) of 0.03wt%.Wherein, level-one pitch can as the raw material of waterproof roll modified pitch,
Two level pitch can be as the raw material of carbon fiber as the raw material of binder pitch, three-level pitch.
Primary concentration is mutually sent into vacuum drying unit, and recycling obtains the extractant of 36kg/h, can be recycled, obtains
The extract remainder (solid slag) of 114kg/h；Secondary concentration phase and three-level concentration mutually enter vacuum distillation tower together, and recycling obtains 30kg/h
Extractant, can be recycled, extract remainder (solid slag) be 20kg/h.Extract remainder (solid slag) is with coal according to 1:4 mass ratio is matched
The water-coal-slurry that solid concentration is 60wt% is made, is sent into gasification furnace and gasifies.
The yield of level-one pitch, two level pitch and three-level pitch is 47.6wt% in the present embodiment, and the yield of solid slag is
53.6wt%.
Embodiment 3
By coal directly-liquefied residue (250kg/h) and middle distillate from coal liquefaction (120~280 DEG C of fractions, 1000kg/h) in 300L
Stirred tank in mixed, stirred tank is protected using nitrogen, is 0.01MPa in pressure, under 120 DEG C of constant temperature, is extracted
Process is taken, obtains extraction mixture.
By above-mentioned extraction mixture be passed through first-stage centrifugal seperator carry out level-one separation of solid and liquid, centrifuging temperature be 120 DEG C, one
The inlet pressure of grade centrifugal separator is 0.06MPa, centrifuge speed 4000r/min, after level-one detaches, primary concentration
The flow of phase is 170kg/h, and level-one clear liquid total flow is 1080kg/h, and the level-one clear liquid of wherein 700kg/h is sent into two level rotation
Stream separator carries out two level separation of solid and liquid.
In two level separation of solid and liquid process, eddy flow temperature is 120 DEG C, and the inlet pressure of two-stage cyclone separator is 0.6MPa,
After two level cyclonic separation, the flow of secondary concentration phase is 12kg/h, and two level clear liquid flow is 688kg/h, will wherein
The two level clear liquid of 350kg/h is sent into cross-flow filter in three-level and carries out three-level separation of solid and liquid.
In three-level separation of solid and liquid process, separation temperature is 120 DEG C, and the inlet pressure of cross-flow filter is in three-level
0.25MPa, the filter core aperture size of filter is 50nm, and after three-stage filtration, the flow of three-level concentration phase is 28kg/h, three
Grade clear liquid flow is 322kg/h.
The three-level clear liquid of the level-one clear liquid of remaining 380kg/h, the two level clear liquid of 338kg/h and 332kg/h is sent respectively
Enter vacuum distillation tower, recovered overhead extractant (middle distillate from coal liquefaction) recycles, and bottom of towe is collected into respectively：Softening point is 147
DEG C, the level-one pitch (41kg/h) that volatile matter content 44.1wt%, ash content are 1.3wt%, softening point is 130 DEG C, volatile matter
The two level pitch (39kg/h) and softening point that content is 53.6wt%, ash content is 0.4wt% are 99 DEG C, and volatile matter content is
61.2wt%, the three-level pitch (30kg/h) that ash content is 0.02wt%.Wherein, level-one pitch can be used as waterproof roll modified pitch
Raw material；Two level pitch can be as the raw material of carbon fiber as the raw material of binder pitch, three-level pitch.
Primary concentration is mutually sent into vacuum drying unit, and recycling obtains the extractant of 45kg/h, can be recycled, obtains
The extract remainder (solid slag) of 125kg/h；Secondary concentration phase and three-level concentration mutually enter vacuum distillation tower together, and recycling obtains 25kg/h
Extractant, can be recycled, extract remainder (solid slag) be 15kg/h.Extract remainder (solid slag) is with coal according to 1:2 mass ratio is matched
The water-coal-slurry that solid concentration is 71wt% is made, is sent into gasification furnace and gasifies.
The yield of level-one pitch, two level pitch and three-level pitch is 44wt% in the present embodiment, and the yield of solid slag is
56wt%.
Embodiment 4
By coal directly-liquefied residue (250kg/h) and coal tar wash oil (230~300 DEG C of fractions, 2000kg/h) in 1100L
Stirred tank in mix, stirred tank is protected using nitrogen, is 0.01MPa in pressure, under 150 DEG C of constant temperature, extracted
Journey obtains extraction mixture.
By above-mentioned extraction mixture be passed through first-stage centrifugal seperator carry out level-one separation of solid and liquid, centrifuging temperature be 150 DEG C, one
The inlet pressure of grade centrifugal separator is 0.04MPa, centrifuge speed 5000r/min, after level-one detaches, primary concentration
The flow of phase is 150kg/h, and level-one clear liquid total flow is 2100kg/h, by the level-one clear liquid of wherein 1400kg/h be sent into two level from
Centrifugal separator carries out two level separation of solid and liquid.
In two level separation of solid and liquid process, separation temperature is 150 DEG C, and the inlet pressure of two-stage centrifugal seperator is 0.03MPa,
Centrifuge speed is 8000r/min, and after two level separation of solid and liquid, the flow of secondary concentration phase is 200kg/h, two level clear liquid stream
It measures as 1200kg/h, the two level clear liquid of 600kg/h therein is sent into cross-flow filter in three-level carries out three-level separation of solid and liquid.
In three-level separation of solid and liquid process, separation temperature is 150 DEG C, and the inlet pressure of cross-flow filter is in three-level
1.0MPa, the filter core aperture size of filter is 100nm, and after three-stage filtration, the flow of three-level concentration phase is 60kg/h, three
Grade clear liquid flow is 540kg/h.
The three-level clear liquid of the level-one clear liquid of remaining 700kg/h, the two level clear liquid of 600kg/h and 540kg/h is sent respectively
Enter vacuum distillation tower, recovered overhead extractant (washing oil) recycles, and bottom of towe is collected into respectively：Softening point is 170 DEG C, volatilization
Point level-one pitch (47.5.kg/h) that content is 38wt%, ash content is 0.5wt%, softening point are 160 DEG C, and volatile matter content is
42wt%, the two level pitch (43.5kg/h) that ash content is 0.2wt% and softening point are 150 DEG C, volatile matter content 44wt%, ash
It is divided into the three-level pitch (40kg/h) of 0.05wt%.Wherein, level-one pitch can be as the raw material of waterproof roll modified pitch；Two level
Pitch can be as the raw material of needle coke as the raw material of dipping agent bitumen, three-level pitch.
Primary concentration is mutually sent into vacuum drying unit, and recycling obtains the extractant of 45kg/h, can be recycled, obtains
The extract remainder (solid slag, solvent content 5wt%) of 105kg/h；Secondary concentration phase and three-level concentration mutually enter vacuum distillation tower together,
Recycling obtains the extractant of 240kg/h, can be recycled, and extract remainder (solid slag, solvent content 5wt%) is 20kg/h.Raffinate
Object (solid slag) is configured to the water-coal-slurry that solid concentration is 80wt%, is sent into gasification furnace and gasifies.
The yield of level-one pitch, two level pitch and three-level pitch is 52.5wt% in the present embodiment, and the yield of solid slag is
50wt%.
Embodiment 5
Coal directly-liquefied residue (250kg/h) and coal tar methylnaphthalene oil (210~310 DEG C of fractions, 1250kg/h) are existed
It is mixed in the stirred tank of 2000L, stirred tank is protected using nitrogen, is 0.5MPa in pressure, under 200 DEG C of constant temperature, is extracted
Process is taken, obtains extraction mixture.
Above-mentioned extraction mixture is passed through cross-flow filter in level-one and carries out level-one separation of solid and liquid, centrifuging temperature is 200 DEG C,
The inlet pressure of cross-flow filters is 0.5MPa in level-one, and the aperture size of filter core is 50 μm, and after level-one detaches, level-one is dense
The flow of contracting phase is 160kg/h, and level-one clear liquid total flow is 2090kg/h, and the level-one clear liquid of wherein 1300kg/h is sent into two level
Gravity settling device carries out two level separation of solid and liquid.
In two level separation of solid and liquid process, separation temperature is 200 DEG C, pressure 0.03MPa, after two level separation of solid and liquid,
The flow of secondary concentration phase is 220kg/h, and two level clear liquid flow is 1080kg/h, and the two level clear liquid of 600kg/h therein is sent
Enter cross-flow filter in three-level and carry out three-level separation of solid and liquid.
In three-level separation of solid and liquid process, separation temperature is 200 DEG C, and the inlet pressure of cross-flow filter is in three-level
0.3MPa, the filter core aperture size of filter is 20nm, and after three-stage filtration, the flow of three-level concentration phase is 60kg/h, three
Grade clear liquid flow is 540kg/h.
The three-level clear liquid of the level-one clear liquid of remaining 790kg/h, the two level clear liquid of 480kg/h and 540kg/h is sent respectively
Enter vacuum distillation tower, recovered overhead extractant (methylnaphthalene oil) recycles, and bottom of towe is collected into respectively：Softening point for 167 DEG C,
The level-one pitch (43.kg/h) that volatile matter content is 41.3wt%, ash content is 1.25wt%, softening point are 159 DEG C, and volatile matter contains
Measure for 45.7wt%, ash content be 0.27wt% two level pitch (37.kg/h) and softening point be 143 DEG C, volatile matter content is
52.1wt%, the three-level pitch (40kg/h) that ash content is 0.03wt%.Wherein, level-one pitch can be used as waterproof roll modified pitch
Raw material；Two level pitch can be as the raw material of needle coke as the raw material of dipping agent bitumen, three-level pitch.
Primary concentration is mutually sent into microwaves drying unit, and recycling obtains the extractant of 56kg/h, can be recycled, obtains
The extract remainder (solid slag, solvent content 3wt%) of 104kg/h；Secondary concentration phase and three-level concentration mutually enter vacuum distillation tower together,
Recycling obtains the extractant of 240kg/h, can be recycled, and extract remainder (solid slag, solvent content 3wt%) is 30kg/h.Raffinate
Object (solid slag) is configured to the water-coal-slurry that solid concentration is 72.5wt%, is sent into gasification furnace and gasifies.
The yield of level-one pitch, two level pitch and three-level pitch is 48.1wt% in the present embodiment, and the yield of solid slag is
51.6wt%.
Comparative example 1
100kg coal directly-liquefied residues and the first extractants of 500Kg (boiling range is 110 DEG C of ＜) are added to stirred tank
In, and them are sufficiently mixed, fill N2Gas is warming up to 100 DEG C, 30 is stirred with the mixing speed of 100r/min to 1.0MPa
Mixture is obtained after minute.Then pressurization heat filtering is carried out, extraction liquid mixture S1 is obtained, is sent into atmospheric distillation tower, cuts ＜
110 DEG C of fraction, the first extractant of recycling recycle.Bottom of towe obtains heavy coal liquids 18.7Kg, then with other cycles
Hydrogenation plant is sent into after solvent and the oil product mixing of heat treatment by-product.Hydroprocessing conditions are 9.5MPa, 365 DEG C, reaction solution space-time
Speed (LHSV) 1.0h-1, gas liquid ratio 850m3/ t, hydrogenation catalyst are Ni-W/ γ-Al2O3, aromatic carbon rate difference is before and after adding hydrogen
0.06, meet requirement of the direct coal liquefaction process to cycle solvent.
The solid matter that level-one is obtained by extraction and the second extractants of 250Kg (boiling range is 220~260 DEG C) are added to and stirred
It mixes in kettle, is then sufficiently mixed them.Fill N2To 1.5MPa, 150 DEG C are warming up to, is stirred with the mixing speed of 100r/min
It mixes and obtains mixture after forty minutes.Then pressurization heat filtering is carried out, obtains extraction liquid mixture, pressure destilling tower is sent into, cuts 220
~260 DEG C of fraction, for the second extractant of recycling for recycling, bottom of towe obtains bitumen 22.4Kg.It is sent into heat treatment
Unit carries out destructive distillation processing at 440 DEG C, obtains heavy oil content 7.6Kg and be subsequently sent to solvent hydrogenation unit, obtains interphase drip
Green 14.7Kg, light gas 0.1Kg.The quinoline insolubles of mesophase pitch are 2.5wt%, and aromatic carbon rate is 0.80, carbon content
89.5wt%, C/H ratio are 1.68.It can be as the raw material for preparing carbon materials.
The yield of intermediate pitch is 22.4wt%, and its softening point is 300 DEG C, and volatile matter content 20wt%, ash content are
1wt%, the yield of heavy coal liquids is 18.7wt%.The total recovery of mink cell focus and bitumen is relatively low, is 41.1wt%.
Comparative example 2
100kg coal directly-liquefied residues and the first extractants of 400Kg (boiling range is 220~260 DEG C) are added to stirring
In kettle, then it is sufficiently mixed them.Fill N2To 2.0MPa, 180 DEG C are warming up to, is stirred with the mixing speed of 200r/min
Mixture is obtained after 30 minutes.Then pressurization heat filtering is carried out, extraction liquid mixture is obtained, is sent into atmospheric distillation tower, cuts 220
~260 DEG C of fraction, the first extractant of recycling recycle, and bottom of towe obtains extract mixture 44.3Kg.By the extract
Mixture is sufficiently mixed with the second extractants of 300Kg (boiling range is 110 DEG C of ＜), is added in stirred tank.Fill N2 extremely
0.5MPa is warming up to 140 DEG C, and mixture is obtained after twenty minutes with the stirring of the mixing speed of 250r/min, then carry out eddy flow from
The heart detaches, and obtains upper layer of extraction liquid mixture S2, is sent into atmospheric distillation tower, cuts the fraction of 110 DEG C of ＜, and the second extraction of recycling is molten
For recycling, bottom of towe obtains heavy coal liquids 22.2kg for agent.Then it is mixed with other cycle solvents and heat treatment by-product oil product
After be sent into hydrogenation plant, Hydroprocessing conditions 11MPa, reacts liquid hourly space velocity (LHSV) (LHSV) 0.8h by 360 DEG C-1, gas liquid ratio 700m3/
T, hydrogenation catalyst are Co-Mo/ γ-Al2O3, aromatic carbon rate difference is 0.07 before and after adding hydrogen, meets direct coal liquefaction process to cycle
The requirement of solvent.
Eddy flow centrifuges underflow and obtains bitumen 22.1Kg.Thermal treatment unit is sent into, destructive distillation is carried out at 450 DEG C
Processing obtains heavy oil content 5.2Kg and is sent into solvent hydrogenation unit, mesophase pitch 16.8Kg, light gas 0.1Kg.Interphase
The quinoline insolubles of pitch are 2.0wt%, and aromatic carbon rate is 0.81, and carbon content 89.7wt%, C/H ratio can be as preparations for 1.70
The raw material of carbon materials.
The yield of intermediate pitch is 22.1wt%, and its softening point is 275 DEG C, volatile matter content 24.1wt%, ash content
For 1.2wt%, the yield of heavy coal liquids is 22.2wt%.The total recovery of mink cell focus and bitumen is relatively low, is
44.3wt%.
It can be seen from the above description that the above embodiments of the present invention realize following technique effect：Comparative example 1
Low with the pitch product yield obtained in comparative example 2, asphalt softening point is high, and volatile matter is low, thus the exploitation applicability of asphaltic products
It is not strong.And by the processing method provided by the present invention, obtain the different three kinds of drips of softening point, volatile matter and content of ashes
Blueness, these three asphaltic products can be applied in different application scenarios when with different physical property.Compared to comparative example 1 and right
Ratio 2, the processing method provided by the present invention can either be avoided because proposing non-to distillate liquefaction oil and bitumen brings respectively
Of high cost, the insufficient problem of separation, additionally it is possible to which specific asphaltic products are prepared according to application demand.So as to reduce life
The pitch add on yield value in coal liquefaction residue is significantly improved under the premise of production cost, coal liquefaction residue is made more to be integrated, more
Adequately recycle.In addition, the application is handled coal directly-liquefied residue using continuous extraction and separation mode, also
Conducive to realization large-scale industrial production application.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, that is made any repaiies
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of processing method of coal directly-liquefied residue, which is characterized in that including：
The coal directly-liquefied residue is extracted using extractant, obtains extraction mixture；To the extraction mixture
Level-one separation of solid and liquid is carried out, obtains level-one clear liquid and primary concentration phase；The extractant is selected from tetrahydrofuran, furfural, N- first
It is one or more in the group that base pyrrolidones, quinoline, toluene and DCL/Direct coal liquefaction distillate form；
Two level separation of solid and liquid is carried out to the level-one clear liquid of part, obtains two level clear liquid and secondary concentration phase；To remaining institute
It states level-one clear liquid and carries out clear liquid solvent recovery processing, obtain level-one pitch；
Three-level separation of solid and liquid is carried out to the two level clear liquid of part, obtains three-level clear liquid and three-level concentration phase；To remaining institute
It states two level clear liquid and carries out clear liquid solvent recovery processing, obtain two level pitch；And
Clear liquid solvent recovery processing is carried out to whole three-level clear liquids, obtains three-level pitch；
Wherein, the two level coal liquefaction pitch is used as by the level-one asphalt applications in road asphalt and waterproof roll field
The three-level pitch is used to prepare needle coke, Carbon fibe, mesocarbon microspheres or super-activated carbon by impregnating agent and binding agent；
The solid content of the primary concentration phase is 50~80wt%, and the solid content of the secondary concentration phase is 15~50wt%, described three
The solid content of grade concentration phase is 10~45wt%.
2. processing method according to claim 1, which is characterized in that the coal directly-liquefied residue and the extraction is molten
Agent is with weight ratio 1:1~8 mixing, in N2Or inert gas shielding, 0.01~1MPa, carry out under conditions of 30~200 DEG C described in
Extraction process；Wherein, extraction time is 5~60min, and stir speed (S.S.) is 25~150r/min.
3. processing method according to claim 1 or 2, which is characterized in that the level-one separation of solid and liquid, the two level solid-liquid
The method of separation and the three-level separation of solid and liquid separately selected from filtration method, cyclonic separation method, centrifugal separation or is sunk
Partition method drops.
4. processing method according to claim 3, which is characterized in that
When being separated by filtration method described in use, separation temperature is 30~200 DEG C, and pressure is 0.1~1.0MPa；
When using the cyclonic separation method, separation temperature is 30~200 DEG C, and pressure is 0.2~0.6MPa；
When using the centrifugal separation, separation temperature is 30~200 DEG C, and pressure is 0.01~0.05MPa；
When using the sedimentation separation method, separation temperature is 30~200 DEG C, and pressure is 0.01~0.1MPa.
5. processing method according to claim 3, which is characterized in that the method for the clear liquid solvent recovery is steamed for normal pressure
It evaporates, be evaporated under reduced pressure or evaporate.
6. processing method according to claim 5, which is characterized in that by the primary concentration phase, the secondary concentration and
The three-level concentration mutually carries out solvent recovery processing, obtains solid slag.
7. processing method according to claim 6, which is characterized in that solid content >=95wt% in the solid slag.
8. processing method according to claim 6, which is characterized in that by the primary concentration phase, the secondary concentration and
The method that the three-level concentration mutually carries out solvent recovery processing is vacuum distillation, air-distillation, vacuum drying, microwave drying or vapour
It carries.
9. the processing method according to any one of claim 6 to 8, which is characterized in that using weight ratio as 1：0~5, by institute
It states solid slag and prepares the water-coal-slurry that solid content is 50~80wt% with coal, then the water-coal-slurry is gasified and burnt.
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| CN105754630A (en) * | 2016-03-25 | 2016-07-13 | 神华集团有限责任公司 | Preparation method of coal liquefied asphalt |
| CN108774547B (en) * | 2018-05-02 | 2021-05-11 | 国家能源投资集团有限责任公司 | System and method for preparing synthesis gas from coal liquefaction residues |
| CN108977222B (en) * | 2018-07-23 | 2021-04-16 | 国家能源投资集团有限责任公司 | Separation system and separation method for direct coal liquefaction oil residue |
| CN109401776B (en) * | 2018-09-30 | 2020-12-01 | 中国科学院山西煤炭化学研究所 | Method and device for high-temperature thermal extraction of asphalt |
| CN110129082A (en) * | 2019-04-12 | 2019-08-16 | 北京中科诚毅科技发展有限公司 | It is a kind of to prepare pitch technique using putty slag |
| CN110295053A (en) * | 2019-08-12 | 2019-10-01 | 胜帮科技股份有限公司 | A kind of recycling processing method of coal chemical industry oil-containing solid slag |
| CN111410982A (en) * | 2020-04-13 | 2020-07-14 | 胜帮科技股份有限公司 | Oil residue fractional separation full-recycling system |
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| CN101962561A (en) * | 2010-09-29 | 2011-02-02 | 神华集团有限责任公司 | Extraction method of direct coal liquefaction residues and application of extracts |
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