CN104845652A - Treatment method for direct coal liquefaction residues - Google Patents
Treatment method for direct coal liquefaction residues Download PDFInfo
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- CN104845652A CN104845652A CN201510317246.6A CN201510317246A CN104845652A CN 104845652 A CN104845652 A CN 104845652A CN 201510317246 A CN201510317246 A CN 201510317246A CN 104845652 A CN104845652 A CN 104845652A
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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 invention provides a treatment method for direct coal liquefaction residues. The treatment method comprises the following steps: extracting direct coal liquefaction residues with an extraction solvent to obtain an extraction mixture; performing first-stage solid-liquid separation on the extraction mixture to obtain a first-stage clear liquid and a first-stage concentrated phase; performing second-stage solid-liquid separation on a part of or all the first-stage clear liquid to obtain a second-stage clear liquid and a second-stage concentrated phase; performing third-stage solid-liquid separation on a part of or all the second-stage clear liquid to obtain a third-stage clear liquid and a third-stage concentrated phase; performing second-stage solid-liquid separation on a part of the first-stage clear liquid and performing clear liquid solvent recovery treatment on rest of the first-stage clear liquid to obtain first-stage pitch; performing third-stage solid-liquid separation on a part of the second-stage clear liquid and performing clear liquid solvent recovery treatment on rest of the second-stage clear liquid to obtain second-stage pitch; and performing clear liquid solvent recovery treatment on all the third-stage clear liquid to obtain third-stage pitch. By the treatment method disclosed by the invention, three pitch products can be obtained and the added profit value of pitch in the direct coal liquefaction residues can be improved favorably.
Description
Technical field
The present invention relates to coal chemical technology, in particular to a kind for the treatment of process of coal directly-liquefied residue.
Background technology
Coal directly-liquefied residue is the non-targeted product of DCL/Direct coal liquefaction process, accounts for 30% of coal feeding amount.It is the material of a kind of high ash, high-sulfur and high heating value, forms primarily of non-distillate carburetion (normal hexane solvend), pitch (normal hexane insoluble tetrahydrofuran (THF) solvend), unconverted coal and inanimate matter.Non-distillate carburetion (heavy coal liquids) and pitch account for 50% of coal directly-liquefied residue, and primarily of many cyclic condensations aromatic hydrocarbons composition, it has, and aromaticity is high, carbon content is high, easy polymerization or crosslinked feature.Different with the characteristic of petroleum pitch and coal-tar pitch, the bitumen in coal directly-liquefied residue is suitable as the raw material preparing carbon material very much, is the carbon resource of a kind of preciousness and uniqueness; Unconverted coal refers in residue the organic matter being insoluble to tetrahydrofuran (THF), accounts for 30% of residue total amount, has higher calorific value; Inanimate matter is mainly made up of the mineral substance in coal and additional catalyzer, accounts for 20% of residue total amount.
How rationally and efficiency utilization coal directly-liquefied residue is very important problem in coal liquefaction craft.Now, the method of domestic large-scale application coal directly-liquefied residue is that coal directly-liquefied residue and coal are deployed into coal water slurry, prepare synthetic gas and hydrogen as gasification furnace raw material, this have found outlet for coal directly-liquefied residue large-scale application, achieves residue as resources and utilizes.But the utilization of coal directly-liquefied residue, particularly tetrahydrofuran (THF) solvend (bitumen) unrealized high added value wherein, thus cause the unrealized maximization of the economic benefit of DCL/Direct coal liquefaction industry.Soluble part in coal directly-liquefied residue and soluble portion are separated, then respectively above-mentioned two portions is reasonably developed, larger economic benefit and social benefit can be produced.
Publication number is that the Japanese Patent of JPS5984977A provides a kind of method extracting organic matter in liquefied residue, the organic matter (comprising heavy coal liquids and asphaltene) extracting obtained all carries out secondary hydrocracking, obtain light naphtha, thus improve the yield of total body fluid carburetion.But due to the existence of bitumen, the method is easy to the problem producing secondary hydrogenation catalyst inactivation because of carbon deposit.
Publication number is that the Japanese Patent of JPH0130412A provides a kind of method isolating heavy coal liquids and bitumen from coal directly-liquefied residue.The heavy coal liquids of separation is carried out secondary hydrocracking and obtains lightweight liquefaction oil by the method, bitumen is entered gelatin liquefaction unit simultaneously and carries out liquefaction reaction again.The method deposits problem both ways: on the one hand, and because the cut of heavy coal liquids is heavier, aromaticity content is higher, not only require carry out deep hydrogenation, cause hydrogen consumption to increase, and easily cause hydrogenation catalyst because of coking inactivation; On the other hand, when liquefying to isolated bitumen, it is liquefaction effect bad again, but also can cause the ill effect such as deposition, coking in liquefying reactor, and therefore the method can not realize the reasonable efficiency utilization of bitumen again.
Grant number is that the Chinese patent of CN101885976 discloses a kind of method extracting bitumen and liquefaction heavy oil from coal directly-liquefied residue, adopt distillate self-produced in DCL/Direct coal liquefaction process as extraction solvent, by bitumen with liquefaction mink cell focus together with extracting and separating out, adopt the method for destructive distillation again, bitumen and liquefaction heavy oil content are opened, obtain mesophase pitch, after liquefaction mink cell focus appropriateness hydrogenation, return gelatin liquefaction unit.Liquefaction mink cell focus is mainly greater than the fractions consisting of 450 DEG C, stronger with bitumen bonding force, when adopting the method for high temperature carbonization to be separated, cause the heavy oil cracking that liquefies on the one hand, cause asphaltic substances coking on the other hand, and the circulating solvent be difficult to as gelatin liquefaction uses.
Grant number is that the patent of CN101962560A and CN101962561A individually discloses a kind of method utilizing two-stage extraction to extract heavy coal liquids and bitumen from coal directly-liquefied residue, the oil product of two different fractions sections that the method produces with DCL/Direct coal liquefaction process self is for extraction solvent, respectively the extraction of two-stage order is carried out to liquefied residue, obtain heavy coal liquids and bitumen.But the method adopts two-stage extraction and two-stage solid-liquid separation, and thus technical process is complicated, while raw material abstraction solvent source single and price is higher, product yield is lower, and cost is higher, and the bitumen softening temperature obtained is high, volatile matter is low, and product development suitability is not strong.
Existence in view of the above problems, is necessary the treatment process developing a kind of coal directly-liquefied residue, to improve the add on yield value of coal directly-liquefied residue medium pitch class material.
Summary of the invention
Main purpose of the present invention is the treatment process providing a kind of coal directly-liquefied residue, with the problem that the add on yield value solving coal directly-liquefied residue medium pitch class material in prior art is lower, realizes the high-efficiency comprehensive utilization of coal liquefaction residue.
To achieve these goals, one aspect of the invention provides a kind for the treatment of process of coal directly-liquefied residue, and the method comprises: adopt extraction solvent to extract coal directly-liquefied residue, be extracted mixture; One-level solid-liquid separation is carried out to extraction mixture, obtains one-level clear liquid and primary concentration phase; Part or all of one-level clear liquid is carried out secondary solid-liquid separation, obtains secondary clear liquid and secondary concentration phase; Part or all of secondary clear liquid is carried out three grades of solid-liquid separation, obtains three grades of clear liquids and three grades of concentrated phases; Secondary solid-liquid separation is carried out to the one-level clear liquid of part, the process of clear liquid solvent recuperation is carried out to remaining one-level clear liquid, obtains one-level pitch; Three grades of solid-liquid separation are carried out to the secondary clear liquid of part, the process of clear liquid solvent recuperation is carried out to remaining secondary clear liquid, obtains secondary pitch; And the process of clear liquid solvent recuperation is carried out to whole three grades of clear liquids, obtain three grades of pitches.
Further, extraction solvent is selected from one or more in the group of tetrahydrofuran (THF), furfural, N-Methyl pyrrolidone, quinoline, toluene, DCL/Direct coal liquefaction distillate or dead oil composition.
Further, coal directly-liquefied residue is mixed with weight ratio 1:1 ~ 8 with extraction solvent, at N
2or protection of inert gas, 0.01 ~ 1MPa, carry out extraction process under the condition of 30 ~ 200 DEG C; Wherein, extraction time is 5 ~ 60min, and stir speed (S.S.) is 25 ~ 150r/min.
Further, the method for one-level solid-liquid separation, secondary solid-liquid separation and three grades of solid-liquid separation is separately selected from filtration, cyclonic separation method, centrifugal separation or settlement separate method.
Further, when adopt can the filtering separation method of serialization time, separation temperature is 30 ~ 200 DEG C, and pressure is 0.1 ~ 1.0MPa; When adopting cyclonic separation method, separation temperature is 30 ~ 200 DEG C, and pressure is 0.2 ~ 0.6MPa; When adopting centrifugal separation, separation temperature is 30 ~ 200 DEG C, and pressure is 0.01 ~ 0.05MPa; When adopting settlement separate method, separation temperature is 30 ~ 200 DEG C, and pressure is 0.01 ~ 0.1MPa.
Further, the solid content of primary concentration phase is 50 ~ 80wt%, and the solid content of secondary concentration phase is 15 ~ 50wt%, and the solid content of three grades of concentrated phases is 10 ~ 45wt%.
Further, the method for clear liquid solvent recuperation is air distillation, underpressure distillation or evaporation.
Further, by primary concentration phase, secondary concentration and three grades are concentrated carries out solvent recuperation process mutually, obtain solid slag; Preferably, Gu solid content >=95wt% in slag.
Further, be underpressure distillation, air distillation, vacuum-drying, microwave drying or stripping by primary concentration phase, the concentrated methods of carrying out solvent recuperation process mutually of secondary concentration and three grades.
Further, take weight ratio as 1:0 ~ 5, solid slag and coal are mixed with the coal water slurry that solid content is 50 ~ 80wt%, then coal water slurry is carried out gasifying and burning; Preferably, one-level pitch may be used for road bitumen and waterproof roll field; Preferably, secondary pitch can use as soaker and binding agent; Preferably, three grades of pitches may be used for preparing needle coke, Carbon fibe, MCMB or super-activated carbon.
Apply technical scheme of the present invention, the non-distillate carburetion (normal hexane soluble part) that coal directly-liquefied residue comprises is very similar to the character of bitumen (normal hexane insoluble tetrahydrofuran (THF) soluble part), the two is difficult to separate completely, and separation costs is higher, be not suitable for carrying out industrial applications, and the over-all properties of the pitch obtained is poor.And in above-mentioned treatment process provided by the invention, continuous extraction separation has been carried out to coal directly-liquefied residue, after non-distillate carburetion and bitumen are extracted in the lump, respectively continuous three solid-liquid separation process are carried out to extraction mixture, one-level pitch, secondary pitch and three grades of pitches can have been obtained.These three kinds of asphaltic products.es can be applied in different application scenarios because having different physical property.This can either avoid because of propose respectively the cost that non-distillate carburetion and bitumen bring high, be separated insufficient problem, specific asphaltic products. can also be prepared according to application demand.Thus the pitch add on yield value that can significantly improve under the prerequisite reducing production cost in coal liquefaction residue, make coal liquefaction residue obtain more comprehensively, more fully recycling.In addition, the application adopts continuous print extracting and separating mode to process coal directly-liquefied residue, also helps and realizes large-scale industrial production application.
Accompanying drawing explanation
The Figure of description forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the process flow diagram of the treatment process of coal directly-liquefied residue provided by the invention.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.Below with reference to the accompanying drawings and describe the present invention in detail in conjunction with the embodiments.
As described by background technology part, existing technique is adopted to there is the not high problem of the add on yield value of coal directly-liquefied residue medium pitch class material.In order to address this problem, the invention provides a kind for the treatment of process of coal directly-liquefied residue, as shown in Figure 1, this treatment process comprises: adopt extraction solvent to extract coal directly-liquefied residue, be extracted mixture; One-level solid-liquid separation is carried out to extraction mixture, obtains one-level clear liquid and primary concentration phase; Part or all of one-level clear liquid is carried out secondary solid-liquid separation, obtains secondary clear liquid and secondary concentration phase; Part or all of secondary clear liquid is carried out three grades of solid-liquid separation, obtains three grades of clear liquids and three grades of concentrated phases; Secondary solid-liquid separation is carried out to the one-level clear liquid of part, the process of clear liquid solvent recuperation is carried out to residue one-level clear liquid, obtains one-level pitch; Three grades of solid-liquid separation are carried out to the secondary clear liquid of part, the process of clear liquid solvent recuperation is carried out to remaining secondary clear liquid, obtains secondary pitch; And the process of clear liquid solvent recuperation is carried out to whole three grades of clear liquids, obtain three grades of pitches.
In the present invention, one-level clear liquid can be divided into various ways process according to demand: partly or entirely one-level clear liquid carries out the process of clear liquid solvent recuperation, and the one-level clear liquid of remainder carries out the process of secondary solid-liquid separation, also all can carry out secondary solid-liquid separation for one-level clear liquid; Similarly, secondary clear liquid can be divided into various ways to process: partly or entirely secondary clear liquid carries out the process of clear liquid solvent recuperation, and the secondary clear liquid of remainder carries out three grades of solid-liquid separation process, also can carry out three grades of solid-liquid separation for all second-order clear liquid.According to the demand of one-level, secondary and three grades of pitches, regulate the process allocation proportion of one-level clear liquid, secondary clear liquid.
The non-distillate carburetion (normal hexane soluble part) that coal directly-liquefied residue comprises is very similar to the character of bitumen (normal hexane insoluble tetrahydrofuran (THF) soluble part), the two is difficult to separate completely, and separation costs is higher, be not suitable for carrying out industrial applications, and the over-all properties of the pitch obtained is poor.And in above-mentioned treatment process provided by the invention, continuous extraction separation has been carried out to coal directly-liquefied residue, after non-distillate carburetion and bitumen are extracted in the lump, respectively continuous three solid-liquid separation process are carried out to extraction mixture, one-level pitch, secondary pitch and three grades of pitches can have been obtained.These three kinds of asphaltic products.es can be applied in different application scenarios because having different physical property.This can either avoid because of propose respectively the cost that non-distillate carburetion and bitumen bring high, be separated insufficient problem, specific asphaltic products. can also be prepared according to application demand.Thus the pitch add on yield value that can significantly improve under the prerequisite reducing production cost in coal liquefaction residue, make coal liquefaction residue obtain more comprehensively, more fully recycling.In addition, the application adopts continuous print extracting and separating mode to process coal directly-liquefied residue, also helps and realizes large-scale industrial production application.
Specifically, the softening temperature of the one-level pitch obtained by above-mentioned treatment process is 120 DEG C ~ 170 DEG C, and volatile content is 30 ~ 50wt%, and ash oontent is 0.5 ~ 5wt%; The softening temperature of secondary pitch is 100 ~ 160 DEG C, and volatile content is 40 ~ 60wt%, and ash oontent is 0.2 ~ 0.5wt%; The softening temperature of three grades of pitches is 85 ~ 150 DEG C, and volatile content is 42 ~ 65wt%, ash oontent <0.1wt%.This shows in solid-liquid separation process, the different in kind of the isolated pitch of different steps, this is conducive to user and selects rational use-pattern according to the different properties of pitch, thus improve the add on yield of coal directly-liquefied residue medium pitch class material, and then improve the economic benefit of whole technique.
In addition, the application adopts multistage solid-liquid separation, clear liquid solvent recuperation repeatedly and carries out solvent recovery operation mutually to concentrated, and this can realize recycling of extraction solvent in coal directly-liquefied residue sepn process, improves the yield of product; Above-mentioned pitch can come into operation without the need to carrying out further deep processing simultaneously, and it is simple that the treatment process that thus the application provides has operating procedure, the advantages such as cost is lower.
In above-mentioned treatment process, the organic solvent that extraction solvent can adopt this area conventional.In one preferably embodiment, in step S1, extraction solvent include but not limited in the group that tetrahydrofuran (THF), furfural, N-Methyl pyrrolidone, quinoline, toluene, DCL/Direct coal liquefaction distillate or dead oil form one or more.Term " DCL/Direct coal liquefaction distillate " can be the distillate of coal direct liquefaction oil in arbitrary fraction section, and term " dead oil " can be the distillate of coal tar in arbitrary fraction section simultaneously.Adopt above-mentioned solvent to be conducive to the solubleness of the bitumen improved in coal directly-liquefied residue, thus improve the productive rate of pitch, the final add on yield improving coal directly-liquefied residue medium pitch class material.
In above-mentioned treatment process, extraction process can adopt conventional operational condition.In one preferably embodiment, coal directly-liquefied residue is mixed with weight ratio 1:1 ~ 8 with extraction solvent, at N
2or protection of inert gas, extract under the condition of 0.01 ~ 1MPa and 30 ~ 200 DEG C, extraction time is 5 ~ 60min, and stir speed (S.S.) is 25 ~ 150r/min.Adopt above-mentioned extraction conditions to be conducive to improving further the productive rate of extraction mixture, and then improve the add on yield of coal directly-liquefied residue medium pitch class material further.Lower-cost mesolow water vapor can be adopted in above-mentioned extraction process to be incubated.
In above-mentioned treatment process, those skilled in the art can select the method for solid-liquid separation.In one preferably embodiment, the method for one-level solid-liquid separation, secondary solid-liquid separation and three grades of solid-liquid separation is separately selected from filtration method, cyclonic separation method, centrifugal separation or settlement separate method.The method of above-mentioned solid-liquid separation is adopted to be conducive to improving the separation efficiency of one-level solid-liquid separation, secondary solid-liquid separation and three grades of solid-liquid separation processes.
In above-mentioned treatment process, those skilled in the art can select the temperature and pressure of solid-liquid separation.In one preferably embodiment, when adopting filtration method, separation temperature is 30 ~ 200 DEG C, and separating pressure is 0.1 ~ 1.0MPa; When adopting cyclonic separation method, separation temperature is 30 ~ 200 DEG C, and inlet pressure is 0.2 ~ 0.6MPa; When adopting centrifugal separation, separation temperature is 30 ~ 200 DEG C, and separating pressure is 0.01 ~ 0.05MPa; When adopting settlement separate method, the temperature of separation is 30 ~ 200 DEG C, and pressure is 0.01 ~ 0.1MPa.Adopt above-mentioned separation temperature to be separated, be conducive to the viscosity reducing extraction mixed solution, thus improve separation efficiency further.Simultaneously according to different solid-liquid isolation methods, different pressure is adopted to be conducive to improving the efficiency be separated further.
In above-mentioned treatment process, those skilled in the art can select respectively primary concentration phase, secondary concentration phase and three grades concentrated mutually in the content of solid content and solvents.In one preferably embodiment, the solid content of primary concentration phase is 50 ~ 80wt%, and the solid content of secondary concentration phase is 15 ~ 50wt%, and the solid content of three grades of concentrated phases is 10 ~ 45wt%.By concentrated to primary concentration phase, secondary concentration phase and three grades mutually in the content of solid content and solvents be each defined in above-mentioned scope and be conducive to improving solid-liquid separation efficiency, shorten the solvent recuperation time simultaneously.
In above-mentioned treatment process, those skilled in the art can select the clear liquid obtained solid-liquid separation process to carry out the method for solvent recuperation.In one preferably embodiment, the method for clear liquid solvent recuperation comprises air distillation, underpressure distillation or evaporation.Adopt aforesaid method to be conducive to improving the organic efficiency of solvent, thus be conducive to the utilising efficiency improving solvent further, reduce the cost of coal directly-liquefied residue treatment process.
In a preferred embodiment, by primary concentration phase, secondary concentration and three grades are concentrated carries out solvent recuperation process mutually, obtain solid slag.This is conducive to obtaining those skilled in the art and rationally applies according to actual needs.Preferably, Gu solid content >=95wt% in slag.Solid content in solid slag is limited in above-mentioned scope, is conducive to the recovery utilization rate improving solvent.
In above-mentioned treatment process, those skilled in the art can select the concentrated method of carrying out solvent recuperation mutually obtained solid-liquid separation process.In a preferred embodiment, primary concentration phase, secondary concentration and three grades of concentrated methods of carrying out solvent recuperation process are mutually included but not limited to underpressure distillation, air distillation, vacuum-drying, microwave drying or stripping.Adopt aforesaid method to be conducive to improving the organic efficiency of solvent, thus be conducive to the utilising efficiency improving solvent further, reduce the cost of coal directly-liquefied residue treatment process.
In above-mentioned treatment process, Gu the Application way of slag can adopt the mode of this area routine.In one preferably embodiment, take weight ratio as 1:0 ~ 5, solid slag and coal are mixed with the coal water slurry that solid content is 50 ~ 80wt%, then above-mentioned coal water slurry is carried out gasifying and burning.With aforementioned proportion, solid slag and coal are mixed with the laggard promoting the circulation of qiization of coal water slurry and are conducive to improving the utilising efficiency of solid slag with burning.Preferably, by one-level asphalt applications in road bitumen and waterproof roll field.Preferably, secondary gelatin liquefaction pitch is used as soaker and binding agent; Preferably, by three grades of pitches for the preparation of needle coke, Carbon fibe, MCMB or super-activated carbon.The output of above-mentioned three kinds of different sorts pitches is conducive to the add on yield further improving coal directly-liquefied residue medium pitch class material, and then improves the economic benefit of whole technique.
Be described in further detail the present invention below in conjunction with specific embodiment, these embodiments can not be interpreted as restriction the present invention scope required for protection.
Embodiment 1
Coal directly-liquefied residue (300kg/h) is mixed in the stirring tank of 50L with tetrahydrofuran (THF) (300kg/h); stirring tank adopts nitrogen to protect, and is 0.02MPa, under 60 DEG C of constant temperature at pressure; carry out extraction process, be extracted mixture.
Above-mentioned extraction mixture is entered primary cyclone and carries out one-level solid-liquid separation, eddy flow temperature is 60 DEG C, and the inlet pressure of primary cyclone is 0.2MPa; After one-level solid-liquid separation, the flow of primary concentration phase is 185kg/h, and one-level clear liquid total flux is 415kg/h, is sent into cross-flow filter in secondary the one-level stillness of night of wherein 265kg/h and carries out secondary solid-liquid separation.
In secondary solid-liquid separation process, separation temperature is 60 DEG C, in secondary, the inlet pressure of cross-flow filter is 0.2MPa, the filter core aperture size of strainer is 2 μm, after cascade filtration, the flow of secondary concentration phase is 21kg/h, and secondary clear liquid flow is 244kg/h, the secondary clear liquid of 120kg/h is wherein sent into cross-flow filter in three grades and carries out three grades of solid-liquid separation.
In three grades of solid-liquid separation processes, separation temperature is 60 DEG C, and in three grades, the inlet pressure of cross-flow filter is 0.18MPa, the filter core aperture size of strainer is 50nm, after three-stage filtration, the flow of three grades of concentrated phases is 12kg/h, and three grades of clear liquid flows are 108kg/h.
By the one-level clear liquid of remaining 150kg/h, the secondary clear liquid of 124kg/h and three grades of clear liquids of 108kg/h send into vacuum still respectively, recovered overhead extraction solvent (tetrahydrofuran (THF)) carries out recycle, collect respectively at the bottom of tower: softening temperature is 120 DEG C, volatile content is 50wt%, ash content is the one-level pitch (56.kg/h) of 4.8wt%, softening temperature is 100 DEG C, volatile content is 60wt%, ash content is the secondary pitch (45kg/h) of 0.28wt% and softening temperature is 85 DEG C, volatile content is 65wt%, ash content is three grades of pitches (40.kg/h) of 0.05wt%.Wherein, one-level pitch can be used as the properties-correcting agent of road bitumen, and secondary pitch can be used as the raw material of dipping agent bitumen, and three grades of pitches can be used as the raw material of needle coke.
Primary concentration sends into vacuum-drying unit mutually, and reclaim the extraction solvent obtaining 35.5kg/h, reusable edible, obtains the extract remainder (Gu slag) of 149.5kg/h; Secondary concentration phase enters atmospheric distillation tower together with three grades of concentrated phases, and reclaim the extraction solvent obtaining 24kg/h, can be recycled, extract remainder (Gu slag) is 9kg/h.Extract remainder (Gu slag) and coal are mixed with according to the mass ratio of 1:5 the coal water slurry that solids concn is 50wt%, send into vapourizing furnace and gasify.
In the present embodiment, the total recovery of one-level pitch, secondary pitch and three grades of pitches is 47.16wt%, Gu the yield of slag is 52.84wt%.
Embodiment 2
Mixed in the stirring tank of 120L with quinoline (500kg/h) by coal directly-liquefied residue (250kg/h), stirring tank adopts nitrogen to protect, and is 0.01MPa, under 100 DEG C of constant temperature, carries out extraction process, be extracted mixture at pressure.
Above-mentioned extraction mixture is passed into first-stage centrifugal separating machine and carries out one-level solid-liquid separation, centrifuging temperature is 100 DEG C, the inlet pressure of first-stage centrifugal separating machine is 0.05MPa, centrifuge speed is 3000r/min, after one-level solid-liquid separation, the flow of primary concentration phase is 150kg/h, and one-level clear liquid total flux is 600kg/h, the one-level clear liquid of wherein 400kg/h is sent into two-stage centrifugal separating machine and carries out secondary solid-liquid separation.
In secondary solid-liquid separation process, separation temperature is 100 DEG C, the inlet pressure of two-stage centrifugal separating machine is 0.04MPa, centrifuge speed is 7000r/min, after secondary solid-liquid separation, the flow of secondary concentration phase is 28kg/h, and secondary clear liquid flow is 372kg/h, the secondary clear liquid of 200kg/h is wherein sent into cross-flow filter in three grades and carries out three grades of solid-liquid separation.
In three grades of solid-liquid separation processes, separation temperature is 100 DEG C, and in three grades, the inlet pressure of cross-flow filter is 0.3MPa, the filter core aperture size of strainer is 20nm, after three-stage filtration, the flow of three grades of concentrated phases is 20kg/h, and three grades of clear liquid flows are 180kg/h.
By the one-level clear liquid of remaining 200kg/h, the secondary clear liquid of 172kg/h and three grades of clear liquids of 120kg/h send into vacuum still respectively, recovered overhead extraction solvent (quinoline) recycle, collect respectively at the bottom of tower: softening temperature is 151 DEG C, volatile content is 42.wt%, ash content is the one-level pitch (46kg/h) of 4.2wt%, softening temperature is 137 DEG C, volatile content is 48wt%, ash content is the secondary pitch (39.kg/h) of 0.35wt% and softening temperature is 109 DEG C, volatile content is 55wt%, ash content is three grades of pitches (34.kg/h) of 0.03wt%.Wherein, one-level pitch can be used as the raw material of waterproof roll modifying asphalt, and secondary pitch can be used as the raw material of binder pitch, and three grades of pitches can be used as the raw material of carbon fiber.
Primary concentration sends into vacuum-drying unit mutually, and reclaim the extraction solvent obtaining 36kg/h, reusable edible, obtains the extract remainder (Gu slag) of 114kg/h; Secondary concentration phase enters vacuum still together with three grades of concentrated phases, and reclaim the extraction solvent obtaining 30kg/h, can be recycled, extract remainder (Gu slag) is 20kg/h.Extract remainder (Gu slag) and coal are mixed with according to the mass ratio of 1:4 the coal water slurry that solids concn is 60wt%, send into vapourizing furnace and gasify.
In the present embodiment, the yield of one-level pitch, secondary pitch and three grades of pitches is 47.6wt%, Gu the yield of slag is 53.6wt%.
Embodiment 3
By coal directly-liquefied residue (250kg/h) and middle distillate from coal liquefaction (120 ~ 280 DEG C of cuts; 1000kg/h) mix in the stirring tank of 300L; stirring tank adopts nitrogen to protect; be 0.01MPa at pressure; under 120 DEG C of constant temperature; carry out extraction process, be extracted mixture.
Above-mentioned extraction mixture is passed into first-stage centrifugal separating machine and carries out one-level solid-liquid separation, centrifuging temperature is 120 DEG C, the inlet pressure of first-stage centrifugal separating machine is 0.06MPa, centrifuge speed is 4000r/min, after flash trapping stage, the flow of primary concentration phase is 170kg/h, and one-level clear liquid total flux is 1080kg/h, the one-level clear liquid of wherein 700kg/h is sent into two-stage cyclone separator and carries out secondary solid-liquid separation.
In secondary solid-liquid separation process, eddy flow temperature is 120 DEG C, the inlet pressure of two-stage cyclone separator is 0.6MPa, after secondary cyclonic separation, the flow of secondary concentration phase is 12kg/h, secondary clear liquid flow is 688kg/h, the wherein secondary clear liquid of 350kg/h is sent into cross-flow filter in three grades and carries out three grades of solid-liquid separation.
In three grades of solid-liquid separation processes, separation temperature is 120 DEG C, and in three grades, the inlet pressure of cross-flow filter is 0.25MPa, the filter core aperture size of strainer is 50nm, after three-stage filtration, the flow of three grades of concentrated phases is 28kg/h, and three grades of clear liquid flows are 322kg/h.
By the one-level clear liquid of remaining 380kg/h, the secondary clear liquid of 338kg/h and three grades of clear liquids of 332kg/h send into vacuum still respectively, recovered overhead extraction solvent (middle distillate from coal liquefaction) recycle, collect respectively at the bottom of tower: softening temperature is 147 DEG C, volatile content is 44.1wt%, ash content is the one-level pitch (41kg/h) of 1.3wt%, softening temperature is 130 DEG C, volatile content is 53.6wt%, ash content is the secondary pitch (39kg/h) of 0.4wt% and softening temperature is 99 DEG C, volatile content is 61.2wt%, ash content is three grades of pitches (30kg/h) of 0.02wt%.Wherein, one-level pitch can be used as the raw material of waterproof roll modifying asphalt; Secondary pitch can be used as the raw material of binder pitch, and three grades of pitches can be used as the raw material of carbon fiber.
Primary concentration sends into vacuum-drying unit mutually, and reclaim the extraction solvent obtaining 45kg/h, reusable edible, obtains the extract remainder (Gu slag) of 125kg/h; Secondary concentration phase enters vacuum still together with three grades of concentrated phases, and reclaim the extraction solvent obtaining 25kg/h, can be recycled, extract remainder (Gu slag) is 15kg/h.Extract remainder (Gu slag) and coal are mixed with according to the mass ratio of 1:2 the coal water slurry that solids concn is 71wt%, send into vapourizing furnace and gasify.
In the present embodiment, the yield of one-level pitch, secondary pitch and three grades of pitches is 44wt%, Gu the yield of slag is 56wt%.
Embodiment 4
By coal directly-liquefied residue (250kg/h) and coal tar wash oil (230 ~ 300 DEG C of cuts; 2000kg/h) mix in the stirring tank of 1100L; stirring tank adopts nitrogen to protect; be 0.01MPa at pressure; under 150 DEG C of constant temperature; carry out extraction process, be extracted mixture.
Above-mentioned extraction mixture is passed into first-stage centrifugal separating machine and carries out one-level solid-liquid separation, centrifuging temperature is 150 DEG C, the inlet pressure of first-stage centrifugal separating machine is 0.04MPa, centrifuge speed is 5000r/min, after flash trapping stage, the flow of primary concentration phase is 150kg/h, and one-level clear liquid total flux is 2100kg/h, the one-level clear liquid of wherein 1400kg/h is sent into two-stage centrifugal separating machine and carries out secondary solid-liquid separation.
In secondary solid-liquid separation process, separation temperature is 150 DEG C, the inlet pressure of two-stage centrifugal separating machine is 0.03MPa, centrifuge speed is 8000r/min, after secondary solid-liquid separation, the flow of secondary concentration phase is 200kg/h, and secondary clear liquid flow is 1200kg/h, the secondary clear liquid of 600kg/h is wherein sent into cross-flow filter in three grades and carries out three grades of solid-liquid separation.
In three grades of solid-liquid separation processes, separation temperature is 150 DEG C, and in three grades, the inlet pressure of cross-flow filter is 1.0MPa, the filter core aperture size of strainer is 100nm, after three-stage filtration, the flow of three grades of concentrated phases is 60kg/h, and three grades of clear liquid flows are 540kg/h.
By the one-level clear liquid of remaining 700kg/h, the secondary clear liquid of 600kg/h and three grades of clear liquids of 540kg/h send into vacuum still respectively, recovered overhead extraction solvent (washing oil) recycle, collect respectively at the bottom of tower: softening temperature is 170 DEG C, volatile content is 38wt%, ash content is the one-level pitch (47.5.kg/h) of 0.5wt%, softening temperature is 160 DEG C, volatile content is 42wt%, ash content is the secondary pitch (43.5kg/h) of 0.2wt% and softening temperature is 150 DEG C, volatile content is 44wt%, ash content is three grades of pitches (40kg/h) of 0.05wt%.Wherein, one-level pitch can be used as the raw material of waterproof roll modifying asphalt; Secondary pitch can be used as the raw material of dipping agent bitumen, and three grades of pitches can be used as the raw material of needle coke.
Primary concentration sends into vacuum-drying unit mutually, and reclaim the extraction solvent obtaining 45kg/h, reusable edible, obtains the extract remainder (Gu slag, solvent 5wt%) of 105kg/h; Secondary concentration phase enters vacuum still together with three grades of concentrated phases, and reclaim the extraction solvent obtaining 240kg/h, can be recycled, extract remainder (Gu slag, solvent 5wt%) is 20kg/h.Extract remainder (Gu slag) is mixed with the coal water slurry that solids concn is 80wt%, sends into vapourizing furnace and gasifies.
In the present embodiment, the yield of one-level pitch, secondary pitch and three grades of pitches is 52.5wt%, Gu the yield of slag is 50wt%.
Embodiment 5
By coal directly-liquefied residue (250kg/h) and coal tar methylnaphthalene oil (210 ~ 310 DEG C of cuts; 1250kg/h) mix in the stirring tank of 2000L; stirring tank adopts nitrogen to protect; be 0.5MPa at pressure; under 200 DEG C of constant temperature; carry out extraction process, be extracted mixture.
Above-mentioned extraction mixture is passed into cross-flow filter in one-level and carries out one-level solid-liquid separation, centrifuging temperature is 200 DEG C, in one-level, the inlet pressure of cross-flow filters is 0.5MPa, the aperture size of filter core is 50 μm, after flash trapping stage, the flow of primary concentration phase is 160kg/h, and one-level clear liquid total flux is 2090kg/h, the one-level clear liquid of wherein 1300kg/h is sent into secondary gravity settling device and carries out secondary solid-liquid separation.
In secondary solid-liquid separation process, separation temperature is 200 DEG C, pressure is 0.03MPa, after secondary solid-liquid separation, the flow of secondary concentration phase is 220kg/h, secondary clear liquid flow is 1080kg/h, the secondary clear liquid of 600kg/h is wherein sent into cross-flow filter in three grades and carries out three grades of solid-liquid separation.
In three grades of solid-liquid separation processes, separation temperature is 200 DEG C, and in three grades, the inlet pressure of cross-flow filter is 0.3MPa, the filter core aperture size of strainer is 20nm, after three-stage filtration, the flow of three grades of concentrated phases is 60kg/h, and three grades of clear liquid flows are 540kg/h.
By the one-level clear liquid of remaining 790kg/h, the secondary clear liquid of 480kg/h and three grades of clear liquids of 540kg/h send into vacuum still respectively, recovered overhead extraction solvent (methylnaphthalene oil) recycle, collect respectively at the bottom of tower: softening temperature is 167 DEG C, volatile content is 41.3wt%, ash content is the one-level pitch (43.kg/h) of 1.25wt%, softening temperature is 159 DEG C, volatile content is 45.7wt%, ash content is the secondary pitch (37.kg/h) of 0.27wt% and softening temperature is 143 DEG C, volatile content is 52.1wt%, ash content is three grades of pitches (40kg/h) of 0.03wt%.Wherein, one-level pitch can be used as the raw material of waterproof roll modifying asphalt; Secondary pitch can be used as the raw material of dipping agent bitumen, and three grades of pitches can be used as the raw material of needle coke.
Primary concentration sends into microwaves drying unit mutually, and reclaim the extraction solvent obtaining 56kg/h, reusable edible, obtains the extract remainder (Gu slag, solvent 3wt%) of 104kg/h; Secondary concentration phase enters vacuum still together with three grades of concentrated phases, and reclaim the extraction solvent obtaining 240kg/h, can be recycled, extract remainder (Gu slag, solvent 3wt%) is 30kg/h.Extract remainder (Gu slag) is mixed with the coal water slurry that solids concn is 72.5wt%, sends into vapourizing furnace and gasifies.
In the present embodiment, the yield of one-level pitch, secondary pitch and three grades of pitches is 48.1wt%, Gu the yield of slag is 51.6wt%.
Comparative example 1
100kg coal directly-liquefied residue and 500Kg first extraction solvent (boiling range is < 110 DEG C) are joined in stirring tank, and makes them fully mix, fill N
2gas, to 1.0MPa, is warming up to 100 DEG C, obtains mixture after stirring 30 minutes with the stirring velocity of 100r/min.Then carry out pressurized heat filtration, be extracted liquid mixture S1, send into atmospheric distillation tower, cut the fraction of < 110 DEG C, reclaim the first extraction solvent and recycle.Obtain heavy coal liquids 18.7Kg at the bottom of tower, after then mixing with other circulating solvent and thermal treatment by-product oil product, send into hydrogenation unit.Hydroprocessing conditions is 9.5MPa, 365 DEG C, reaction solution hourly space velocity (LHSV) 1.0h
-1, vapour-liquid ratio 850m
3/ t, hydrogenation catalyst is Ni-W/ γ-Al
2o
3, before and after hydrogenation, aromatic carbon rate difference is 0.06, meets the requirement of direct coal liquefaction process to circulating solvent.
One-level is extracted the solid matter obtained and 250Kg second extraction solvent (boiling range is 220 ~ 260 DEG C) joins in stirring tank, then make them fully mix.Fill N
2to 1.5MPa, be warming up to 150 DEG C, after stirring 40 minutes with the stirring velocity of 100r/min, obtain mixture.Then carry out pressurized heat filtration, be extracted liquid mixture, send into pressure distillation tower, cut the fraction of 220 ~ 260 DEG C, reclaiming the second extraction solvent for recycling, at the bottom of tower, obtaining bitumen 22.4Kg.Send into thermal treatment unit, at 440 DEG C, carry out destructive distillation process, obtain heavy oil content 7.6Kg and send into solvent hydrogenation unit subsequently, obtain mesophase pitch 14.7Kg, light gas 0.1Kg.The quinoline insolubles of mesophase pitch is 2.5wt%, and aromatic carbon rate is 0.80, and carbon content 89.5wt%, C/H ratio is 1.68.Can as the raw material preparing carbon materials.
The yield of intermediate pitch is 22.4wt%, and its softening temperature is 300 DEG C, and volatile content is 20wt%, ash content is 1wt%, and the yield of heavy coal liquids is 18.7wt%.The total recovery of mink cell focus and bitumen is lower, is 41.1wt%.
Comparative example 2
100kg coal directly-liquefied residue and 400Kg first extraction solvent (boiling range is 220 ~ 260 DEG C) are joined in stirring tank, then makes them fully mix.Fill N
2to 2.0MPa, be warming up to 180 DEG C, after stirring 30 minutes with the stirring velocity of 200r/min, obtain mixture.Then carry out pressurized heat filtration, be extracted liquid mixture, send into atmospheric distillation tower, cut the fraction of 220 ~ 260 DEG C, reclaim the first extraction solvent and recycle, at the bottom of tower, be extracted thing mixture 44.3Kg.This extract mixture is fully mixed with 300Kg second extraction solvent (boiling range is < 110 DEG C), adds in stirring tank.Fill N2 to 0.5MPa, be warming up to 140 DEG C, mixture is obtained after stirring 20 minutes with the stirring velocity of 250r/min, then eddy flow centrifugation is carried out, obtain upper layer of extraction liquid mixture S2, send into atmospheric distillation tower, cut the fraction of < 110 DEG C, reclaiming the second extraction solvent for recycling, at the bottom of tower, obtaining heavy coal liquids 22.2kg.Then send into hydrogenation unit after mixing with other circulating solvent and thermal treatment by-product oil product, Hydroprocessing conditions is 11MPa, 360 DEG C, reaction solution hourly space velocity (LHSV) 0.8h
-1, vapour-liquid ratio 700m
3/ t, hydrogenation catalyst is Co-Mo/ γ-Al
2o
3, before and after hydrogenation, aromatic carbon rate difference is 0.07, meets the requirement of direct coal liquefaction process to circulating solvent.
Eddy flow centrifugation underflow obtains bitumen 22.1Kg.Send into thermal treatment unit, at 450 DEG C, carry out destructive distillation process, obtain heavy oil content 5.2Kg and send into solvent hydrogenation unit, mesophase pitch 16.8Kg, light gas 0.1Kg.The quinoline insolubles of mesophase pitch is 2.0wt%, and aromatic carbon rate is 0.81, and carbon content 89.7wt%, C/H are than being 1.70 can as the raw material preparing carbon materials.
The yield of intermediate pitch is 22.1wt%, and its softening temperature is 275 DEG C, and volatile content is 24.1wt%, ash content is 1.2wt%, and the yield of heavy coal liquids is 22.2wt%.The total recovery of mink cell focus and bitumen is lower, is 44.3wt%.
As can be seen from the above description, the above embodiments of the present invention achieve following technique effect: the pitch product yield obtained in comparative example 1 and comparative example 2 is low, and pitch softening point is high, and volatile matter is low, and thus the exploitation suitability of asphaltic products. is not strong.And by treatment process provided by the invention, obtaining three kinds of pitches that softening temperature, volatile matter and ash oontent are all not identical, these three kinds of asphaltic products.es can be applied in different application scenarios because having different physical property.Compared to comparative example 1 and comparative example 2, treatment process provided by the invention can either avoid because of propose respectively the cost that non-distillate carburetion and bitumen bring high, be separated insufficient problem, specific asphaltic products. can also be prepared according to application demand.Thus the pitch add on yield value that can significantly improve under the prerequisite reducing production cost in coal liquefaction residue, make coal liquefaction residue obtain more comprehensively, more fully recycling.In addition, the application adopts continuous print extracting and separating mode to process coal directly-liquefied residue, also helps and realizes large-scale industrial production application.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a treatment process for coal directly-liquefied residue, is characterized in that, comprising:
Adopt extraction solvent to extract described coal directly-liquefied residue, be extracted mixture; One-level solid-liquid separation is carried out to described extraction mixture, obtains one-level clear liquid and primary concentration phase;
Part or all of described one-level clear liquid is carried out secondary solid-liquid separation, obtains secondary clear liquid and secondary concentration phase;
Part or all of described secondary clear liquid is carried out three grades of solid-liquid separation, obtains three grades of clear liquids and three grades of concentrated phases;
Secondary solid-liquid separation is carried out to the described one-level clear liquid of part, the process of clear liquid solvent recuperation is carried out to remaining described one-level clear liquid, obtains one-level pitch;
Three grades of solid-liquid separation are carried out to the described secondary clear liquid of part, the process of clear liquid solvent recuperation is carried out to remaining described secondary clear liquid, obtains secondary pitch; And
The process of clear liquid solvent recuperation is carried out to whole described three grades of clear liquids, obtains three grades of pitches.
2. treatment process according to claim 1, is characterized in that, described extraction solvent be selected from tetrahydrofuran (THF), furfural, N-Methyl pyrrolidone, quinoline, toluene, DCL/Direct coal liquefaction distillate or dead oil composition group in one or more.
3. treatment process according to claim 1 and 2, is characterized in that, mixes, described coal directly-liquefied residue at N with described extraction solvent with weight ratio 1:1 ~ 8
2or protection of inert gas, 0.01 ~ 1MPa, carry out described extraction process under the condition of 30 ~ 200 DEG C; Wherein, extraction time is 5 ~ 60min, and stir speed (S.S.) is 25 ~ 150r/min.
4. treatment process according to any one of claim 1 to 3, it is characterized in that, the method for described one-level solid-liquid separation, described secondary solid-liquid separation and described three grades of solid-liquid separation is separately selected from filtration method, cyclonic separation method, centrifugal separation or settlement separate method.
5. treatment process according to claim 4, is characterized in that,
When adopting described filtering separation method, separation temperature is 30 ~ 200 DEG C, and pressure is 0.1 ~ 1.0MPa;
When adopting described cyclonic separation method, separation temperature is 30 ~ 200 DEG C, and pressure is 0.2 ~ 0.6MPa;
When adopting described centrifugal separation, separation temperature is 30 ~ 200 DEG C, and pressure is 0.01 ~ 0.05MPa;
When adopting described settlement separate method, separation temperature is 30 ~ 200 DEG C, and pressure is 0.01 ~ 0.1MPa.
6. treatment process according to claim 5, is characterized in that, the solid content of described primary concentration phase is 50 ~ 80wt%, and the solid content of described secondary concentration phase is 15 ~ 50wt%, and the solid content of described three grades of concentrated phases is 10 ~ 45wt%.
7. treatment process according to claim 4, is characterized in that, the method for described clear liquid solvent recuperation is air distillation, underpressure distillation or evaporation.
8. treatment process according to claim 7, is characterized in that, described primary concentration phase, described secondary concentration and described three grades concentrated is carried out solvent recuperation process mutually, obtains solid slag; Preferably, the solid content >=95wt% in described solid slag.
9. treatment process according to claim 8, is characterized in that, is underpressure distillation, air distillation, vacuum-drying, microwave drying or stripping by described primary concentration phase, described secondary concentration and described three grades of concentrated methods of carrying out solvent recuperation process mutually.
10. treatment process according to claim 8 or claim 9, it is characterized in that, take weight ratio as 1:0 ~ 5, described solid slag and coal prepared the coal water slurry that solid content is 50 ~ 80wt%, then described coal water slurry is carried out gasifying and burning;
Preferably, described one-level pitch may be used for road bitumen and waterproof roll field;
Preferably, described secondary pitch can use as soaker and binding agent;
Preferably, described three grades of pitches may be used for preparing needle coke, Carbon fibe, MCMB or super-activated carbon.
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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 |
| CN108774547A (en) * | 2018-05-02 | 2018-11-09 | 国家能源投资集团有限责任公司 | The system and method for coal liquefaction residue producing synthesis gas |
| CN108977222A (en) * | 2018-07-23 | 2018-12-11 | 国家能源投资集团有限责任公司 | The separation system and separation method of directly liquefying coal into oil residue used |
| CN109401776A (en) * | 2018-09-30 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A kind of method and device of asphalt high-temperature extraction heat |
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| CN103242881A (en) * | 2013-05-30 | 2013-08-14 | 神华集团有限责任公司 | Method for separating bituminous substances from coal direct liquefaction residues |
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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 |
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| 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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