CN102399566A - Method for extracting heavy liquefied oil and kerite substance from residue of direct coal liquefaction - Google Patents
Method for extracting heavy liquefied oil and kerite substance from residue of direct coal liquefaction Download PDFInfo
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Abstract
The invention provides a method for extracting heavy liquefied oil and kerite substances from residues of direct coal liquefaction. The method comprises steps of: a) adding coal residue powder and a first solvent into an extraction apparatus for extraction; b) carrying out solid-liquid separation on an extraction mixture and a raffinate from step a) by a first cyclone separator to obtain a liquid mixture and an underflow mixture; c) sending the underflow mixture from step b) and a second solvent to a re-extraction apparatus for re-extraction to obtain a mixture; d) carrying out a second solid-liquid separation on an extraction mixture and a raffinate from step c) by a second cyclone separator too obtain a liquid mixture and an underflow mixture; e) carrying out precise filtration on a clear liquid mixture from step b) and a re-extracting clear liquid mixture from step e) in a precision filtering device and sending a filtrate to a distillation separator; f) carrying out pressurizing coarse filtration on the underflow mixture from step d) and sending a filtrate part and a clear liquid mixture treated with precise filtration to a distillation separator; g) separating the extraction mixture in the distillation separator.
Description
Technical field
The present invention relates to coal deep processing field, particularly a kind of to the solid-liquid separation after the coal liquefaction residue extraction and the method for solvent recuperation.Specifically, the invention provides a kind of method that from coal directly-liquefied residue, extracts heavy liquefaction oil and bitumen.
Background technology
Coal direct liquefaction is the important supplement to the China's oil shortage of resources, and is significant to Chinese energy safety.No matter adopt which kind of coal direct liquefaction technology, like IGOR
+Technology, NEDOL technology and Shenhua liquefaction process (ZL200410070249.6 and ZL200610090484.9), the transformation efficiency of coal all can not reach 100%, and about 30% the liquefied residue by product that accounts for the liquefaction coal input quantity is always arranged at last.It is a kind of high-carbon, high ash and doctor positive material, and the unconverted coal, asphaltene and the heavy liquefaction oil that mainly exist by the mineral substance in the coal, catalyzer, with solid form are formed.Wherein the heavy liquefaction oil in the residue, bitumen content account for about 50% of level of residue, and unconverted coal accounts for about 30%, and ash content and catalyzer account for about 20%.
Reclaim the heavy oil product in the liquefied residue, to improving the oily yield of whole coal liquefaction craft, the economic benefit of factory improves efficiency of resource thereby raising is liquefied, and reduces energy dissipation and has very important significance.In addition, the bituminous matter in the coal directly-liquefied residue mainly is made up of the polycyclic condensed aromatics, has the aromaticity height; Carbon content is high, and polymerization or crosslinked characteristics have the unexistent characteristic of a lot of petroleum pitch matter easily; Be suitable as very much the raw material of preparation carbon materials; Be a kind of very valuable and unique resource, the bitum application of gelatin liquefaction receives people's attention day by day, is expected to prepare the carbon product of some high added values.It is the method that the prepared using plasma body prepares nano-carbon material with the coal direct liquefaction residue that Chinese patent ZL200510047800.X discloses a kind of.Chinese patent ZL200610012547.9 discloses a kind of with the method for coal liquefaction residue as road asphalt modifier.Chinese patent ZL200910087907.5 discloses a kind of method of utilizing coal directly-liquefied residue to prepare asphalt base carbon fiber.China ZL200910086158.4 discloses a kind of method for preparing mesophase pitch with coal liquefaction residue.These methods all are to be raw material with the bitumen in the coal liquefaction residue; But from residue, do not isolate the heavy liquefaction oil and be used; Caused the waste of oil product resource undoubtedly; And the extracting of residue medium pitch class material all is to be solvent with expensive pure chemistry reagent, and cost is higher relatively, and research at present is in the laboratory lab scale stage basically.
Current large approach that utilizes to coal liquefaction residue mainly contains methods such as burning, coking system oil, gasification hydrogen-producing.Coal liquefaction residue acts as a fuel and directly in boiler or kiln, burns, and will influence the economy of gelatin liquefaction undoubtedly, causes the waste of resource, and higher sulphur content will be brought the problem aspect the environment in the liquefied residue in combustion processes.Coking system oil is that the asphaltene in the liquefied residue is converted into BO and retortable oil; Though can increase the liquid oil yield of coal liquefaction craft to a certain extent; But semi-coke yield is high after the liquefied residue coking; The oil yield is low, and coking obtain the sulphur content of semicoke high with the ash content height, it utilizes approach also very not clear and definite.Patent CN101760220A discloses a kind of method for continuously coking and equipment of coal liquefied residue; Coking operation carries out under high temperature, condition of high vacuum degree; But because high, the polymerization easily of aromaticity content in the heavy liquefaction oil; It is coke that the heavy liquefaction oil polycondensation of significant proportion is arranged when thermal treatment, and therefore the actual BO ratio that obtains is not high.The method of liquefied residue being carried out gasification hydrogen-producing is a kind of effectively extensive approach that utilizes, but the high value added utilization potentiality of bitumen in the residue and BO are not obtained embodying.
About 50% BO, asphaltene etc. in the residue are had the separating substances of higher utility value to come out and carry out comprehensive processing and utilization respectively, make it produce bigger economic benefit, be a challenging subject in DCL/Direct coal liquefaction field always.One of difficult point wherein is the problem of solid-liquid separation and solvent recuperation.Why these problems are difficult to solve is because the characteristics decision of liquefied residue.The grain graininess of solids is very thin in the coal direct liquefaction residue, particle size distribution from less than 1 μ m to several microns, part is suspended in the raffinate, part is colloidal state; Because the existence of high viscosity materials such as asphaltene, asphaltene before in the liquefied residue, and effects such as therein swelling of unconverted coal, peptization can determine that all the viscosity of liquefied residue is very high; Because liquid phase is made up of heavy liquefaction oil and bituminous matter basically, so the density difference between liquid phase and the solid particulate is smaller.All these characteristics have caused the difficulty of liquefied residue solid-liquid separation.JP 1304182 discloses a kind of method of from the direct liquefaction residue, isolating heavy liquefaction oil and bitumen.CN101885976A, CN101962560A and CN101962561A disclose a kind of heavy-fluid carburetion and bituminous matter and comprehensive utilization method in addition respectively of from coal directly-liquefied residue, extracting.The operational path that above patent provides has farthest been brought into play BO and the bitum potentiality of utilizing in the residue, but does not provide concrete solid-liquid separation and extraction solvent recovery scheme.
Inventor's years of researches are found; Select suitable solvent can from liquefied residue, extract heavy liquefaction oil and bitumen, but in the residue extraction process, the residue solid substrate concentration is big; The concentration of common soluble solid particulate matter accounts for 10～40% of extraction system; And, bring very big difficulty for the solid-liquid separation of extraction system because the existence of high-viscosity materials such as bituminous matter makes extraction system viscosity relatively large.Therefore; How to realize extracting the efficient solid-liquid separation of mixture (extraction solvent, liquefaction BO and bituminous matter) and extract remainder (solid part in the residue); Farthest reclaim extraction solvent; Thereby improving the technical and economic feasibility of extraction process, is the main bottleneck of restriction residue abstraction technique development.The domestic and international research achievement does not address this problem effectively at present.Patent JP2289684 adopts the method for gravity settling that the extraction mixture is separated with extract remainder with patent JP61276889; But this method separation efficiency is relatively low; Precipitation apparatus is relatively heavier; The extract ash content that finally obtains is difficult to reach and is lower than 1% requirement, and the extraction solvent loss is bigger.Kerr-McGee company (U.S. Patent number 3,607,716; U.S. Patent number 3,607,717) adopt light aromatics solvent such as toluene etc.; Extraction liquefied residue under super critical condition, solid-liquid separation still adopts the method for gravity settling, although this technology can obtain ash less than 1% extraction product; Solvent recovering rate is higher, but extraction temperature is than higher 325～340 ℃, the big 5.0MPa of pressure ratio; This technology extraction conditions is relatively harsh, and plant energy consumption is high, equipment requirements is high, and settlement separate efficient is not high yet.
Summary of the invention
The present invention proposes a kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen; Purpose is to realize the solid-liquid high efficiency separation of liquefied residue extraction mixture and extract remainder; Obtain the residue extract (comprising heavy liquefaction oil and bitumen) that ash content is lower than 0.1wt%, this extract will become the high quality raw material of high value added product; Simultaneously, present method can farthest reclaim extraction solvent, improves solvent recovering rate, is beneficial to the long-term stability running of implement device, reduces running cost, thereby improves the Technological Economy property of technological process.
A kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen that the present invention proposes; It is characterized in that liquefaction oil (being called first solvent) as extraction solvent, coal directly-liquefied residue is extracted extraction mixture (comprising solvent, extraction heavy liquefaction oil, extraction bituminous matter) and extract remainder to obtain liquefied residue with a kind of specific fraction section.
A kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen that the present invention proposes is characterized in that cyclone separator and filtration unit are coupled, and is used for the solid-liquid separation of liquefied residue extract and extract remainder.Specifically; This method is at first low with cost of investment, safety is high and suitable continuous run in long period and the high cyclone separator of separation efficiency extract the solid-liquid roughing out of mixture and extract remainder; Be directed against the requirement of subsequent technique then; Overflow clear liquid to cyclone separator carries out secondary filter, obtains ash less than 0.1% liquefied residue extract (comprising heavy liquefaction oil and bitumen).
A kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen that the present invention proposes; It is characterized in that; Big to solvent residual amount in the cyclone separator underflow, and in the residue extractable matter not by complete isolating problem, with the liquefaction oil (being called second solvent) of another kind of specific fraction section as extraction solvent; The rotational flow separation underflow is extracted again, and then reclaim solvent and residue extract.
A kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen that the present invention proposes is characterized in that the underflow after second solvent extracts again at first carries out the pressurized raw filtration, reclaims residual solvent and extract; Then filter residue is used the heating agent blowback, carry out drying treatment, further reclaim and residue in the extraction solvent in the filter residue.
According to an aspect of the present invention, a kind of method that from the coal direct liquefaction residue, extracts heavy liquefaction oil and bitumen is provided, has said method comprising the steps of:
A) coal liquefaction residual powder is joined with first solvent carry out thorough mixing extraction in the residue extraction plant, so that comprise heavy liquefaction oil and bitum extractable matter in the liquefied residue are extracted in first solvent;
B) utilize first cyclone separator that comprise first solvent, heavy liquefaction oil, bitum extraction mixture and the residue extract remainder that obtains in the step a) carried out solid-liquid separation, obtain the spissated underflow mixture of clear liquor phase mixture and bottom of upper strata overflow respectively;
C) the spissated underflow mixture in the bottom in the step b) is sent to second solvent again carries out extraction treatment again in the extraction plant, first solvent of carrying secretly in the underflow mixture and extractable matter are extracted in second solvent again, to obtain to extract again mixture;
D) utilize second cyclone separator to comprise first solvent, second solvent, heavy liquefaction oil, bitumly extract mixture again and the residue extract remainder carries out the solid-liquid separation second time, obtain the spissated underflow mixture that extracts again of clear liquor phase mixture of extraction again and bottom of upper strata overflow respectively what obtain in the step c);
E) clear liquor phase mixture in the step b) and the clear liquor of the extraction again phase mixture in the step e) are carried out secondary filter in the secondary filter device, and filtrating is sent in the fractionation by distillation device;
F) the spissated underflow mixture that extracts again in the bottom in the step d) is carried out pressurized raw and filters in the pressurized raw filtration unit, the filtrating part with extract the clear liquor phase mixture again through secondary filter, send into the fractionation by distillation device;
G) in the fractionation by distillation device, the extraction mixture is separated, supply to recycle, and obtain heavy liquefaction oil and ash less than 0.1% bitumen to reclaim first solvent, second solvent.
According to the method for the invention, wherein, said method also comprises step h between step f) and step g)): remaining filter residue carried out drying treatment with the heating agent blowback after pressurized raw was filtered in to step f), reclaimed residual solvent, sent into the fractionation by distillation device.
According to the method for the invention, wherein, said first solvent and second solvent are in the DCL/Direct coal liquefaction process liquefaction oil product that directly produces, and said first solvent is 160～260 ℃ a fraction, and said second solvent is the fraction of over point (IBP)～110 ℃.
According to the method for the invention, wherein, the extracting operation condition in said step a) is: the mass ratio of coal liquefaction residue and said first solvent is 1: 1～10, be preferably 1: 2～and 8; N
2And/or H
2Atmosphere, pressure is 0.1～3.0MPa, is preferably 0.2～2.5MPa; Extraction temperature is 60～300 ℃, is preferably 80～250 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min; The solid concentration of extraction back system is 5～30%, and system density is 0.95～1.5g/ml.
According to the method for the invention; Wherein, At said step b) and d) in extraction mixture and the solid concentration that extracts the clear liquor phase mixture of the upper strata overflow that mixture obtains again after rotational flow separation be 1%～5%, the solid concentration of the spissated underflow mixture in bottom is 40～60%.
According to the method for the invention, wherein, the condition of extracting operation again of second solvent is in said step c): the mass ratio of coal liquefaction residue and said second solvent is 1: 1～10, be preferably 1: 1～and 6; N
2And/or H
2Atmosphere, pressure is 0.2～3.5MPa, is preferably 0.5～2.5MPa; Extraction temperature is 30～250 ℃, is preferably 40～150 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min.
According to the method for the invention, wherein, the clear liquor phase mixture of the upper strata overflow that rotational flow separation obtains in said step e) obtains solid concentration and is not more than 0.01% filtrating after secondary filter.
According to the method for the invention, wherein, the pore size filter of the secondary filter device that in said step e), uses is 0.5～3 μ m.
According to the method for the invention, wherein, the spissated underflow mixture that extracts again obtains solid concentration and is not more than 5% filtrating after pressurized raw is filtered in said step f).
According to the method for the invention, wherein, the pore size filter of the pressurized raw filtration unit that in said step f), uses is 10～50 μ m.
According to the method for the invention, wherein, the solid concentration of pressurized raw filtered filtration residue is 70～90% in said step f).
According to the method for the invention, wherein, at said step h) in heating agent be meant nitrogen, helium rare gas element and water vapor or their mixture, it is heated to 100～300 ℃ in heating unit, be used for the blowback drying treatment of coarse filtration filter residue.
According to the method for the invention, wherein, at said step h) in, reclaim residual solvent and at least one oil-gas separator, carry out.
According to the method for the invention, wherein, in said step g), the fractionation by distillation device is air distillation tripping device, underpressure distillation tripping device or both combinations, preferably both combinations.
According to the method for the invention, wherein, the particle diameter of said coal directly-liquefied residue powder is 0.05～2mm.
According to the method for the invention, wherein, said residue extraction plant and again extraction plant be provided with whipping device and recycle pump.
According to the method for the invention, wherein, said secondary filter device and pressurized raw filtration unit are provided with pressure equipment and blowback air system are provided.
According to another aspect of the present invention, provide a kind of by the heavy liquefaction oil and the bitumen that extract according to preceding method.
The heavy liquefaction oil and the bitumen that extract according to the method for the invention, wherein, the boiling range of said heavy liquefaction oil is 260～450 ℃, the ash of said bitumen is less than 0.1%.
The method that from coal directly-liquefied residue, extracts heavy liquefaction oil and bitumen provided by the invention; Adopt that separation efficiency is high, equipment volume is little, flexible operation, realize that the cyclone separator of long-term operation extracts the solid-liquid separation of mixture and extract remainder easily, and coupling obtains high quality, hangs down the extract (heavy liquefaction oil and bitumen) of ash with secondary filter; Adopt lightweight solvent method of extraction again, improved the percentage extraction and first solvent recovering yield of liquefied residue to greatest extent; Blowback exsiccant method has improved second solvent recovering yield to greatest extent after adopting coarse filtration.This method has solved the difficult problem of solid-liquid separation in the residue abstraction technique, has farthest reclaimed extraction solvent simultaneously, has reduced solvent loss, has realized solvent recycling.This method technological process is simple, workable; Be easy to realize long-term operation; Improved the oily yield of whole liquefaction process; And, avoided the waste of liquefied residue resource for the preparation of carbon materials provides the fine raw material, the whole economic efficiency that improves liquefaction factory is had very important realistic meaning.
Description of drawings
With reference to the accompanying drawings, can be more readily understood technical scheme of the present invention.In the accompanying drawing:
Fig. 1 shows an a kind of schema that extracts the method for heavy liquefaction oil and bitumen from coal directly-liquefied residue.
Embodiment
Below in conjunction with Fig. 1 method provided by the present invention is at length explained, but the present invention is not limited to this.
As shown in Figure 1, the coal directly-liquefied residue powder 1 after the fragmentation and first solvent 2 are joined in the residue extraction plant 3 via first colvent inlet 32 and coal directly-liquefied residue inlet 31 respectively by a certain percentage, under certain extraction conditions, carry out extracting operation.Then; To preferably be pumped into first cyclone separator 4 carrying out solid-liquid separation from the coal liquefaction residue extraction mixture outlet 41 of cyclone separator 4 through the solidliquid mixture of extraction from what the coal liquefaction residue of residue extraction plant 3 extraction mixture outlet 33 was discharged, thereby the height of realizing the gelatin liquefaction solid residue concentrates via topping-up pump.Wherein, Said residue extraction plant 3 also has the residue extraction mixture inlet 34 that is positioned at said residue extraction plant 3 tops; The said coal liquefaction residue extraction mixture outlet 34 of said residue extraction plant 3 is positioned at the bottom of said residue extraction plant 3, and the said coal liquefaction residue extraction mixture outlet 33 of said residue extraction plant 3 also is connected to the said residue extraction mixture inlet 34 on said residue extraction plant 3 tops.Preferably, the clear liquor phase mixture of the upper strata overflow of discharging from the clear liquor phase mixture of first cyclone separator 4 outlet 43 is flow into first storage tank 6, so that regime flow via the liquid inlet of first storage tank 6.Then, will be pressed into the secondary filter device 7 via the clear liquor phase mixture inlet 71 of secondary filter device 7 from the liquid that the liquid exit of first storage tank 6 is discharged.Preferably, the filtrating of discharging from the secondary filter clear filtrate outlet 73 of secondary filter device 7 is flow into second storage tank 8.The spissated underflow mixture in bottom of discharging from the spissated underflow mixture outlet of first cyclone separator 4 42 is flow into the extraction plant 5 via the spissated underflow mixture inlet 51 of extraction plant 5 more again; And by a certain percentage second solvent 19 is joined in the extraction plant 5 via second colvent inlet 52 again, carry out extracting operation more under certain condition.
Then; To preferably be pumped into from the solidliquid mixture of the extraction again inlet 121 of second cyclone separator 12 second cyclone separator 12 carrying out solid-liquid separation from the solidliquid mixture that extracts the extraction again that solidliquid mixture outlet 53 discharges again of extraction plant 5 again, thereby the height of realizing the gelatin liquefaction solid residue concentrates via topping-up pump.Wherein, Said extraction plant again 5 also has the solidliquid mixture of the extraction again inlet 54 that is positioned at said extraction plant again 5 tops; Said extraction plant again 5 said extracts the bottom that solidliquid mixture outlet 53 is positioned at said extraction plant again 5 again, and said extraction plant again 5 said extracts the said solidliquid mixture inlet 54 that extracts again that solidliquid mixture outlet 53 also is connected to said extraction plant again 5 tops again.Preferably; Make from the clear liquor phase mixture that extracts again that extracts upper strata overflow that clear liquor phase mixture outlet 123 discharges again of second cyclone separator 12 to flow into first storage tank 6 via the liquid inlet of first storage tank 6, so that regime flow with the clear liquor phase mixture of the upper strata overflow of discharging from the clear liquor phase mixture outlet 43 of first cyclone separator 4.Then; To be pressed into the secondary filter device 7 via the clear liquor phase mixture inlet 71 of secondary filter device 7 from the liquid that the liquid exit of first storage tank 6 is discharged, the filtrating of discharging from the secondary filter clear filtrate outlet of secondary filter device 7 is flow into second storage tank 8.To extract the spissated underflow mixture that extracts again in bottom that underflow mixture outlet 122 discharges again from second cyclone separator 12 spissated and extract underflow mixture inlet 131 again via pressurized raw filtration unit 13 spissated and flow into the pressurized raw filtration unit 13, and carry out hot pressurized raw and filter.After the filtrating of gained is discharged from the coarse filtration filtrate outlet 132 of pressurized raw filtration unit 13; Get in the secondary filter device 7 via the coarse filtration filtrating inlet 72 of secondary filter device 7; Filtrate filtered flow in second storage tank 8 via the secondary filter clear filtrate outlet 73 of secondary filter device 7, so that regime flow.
Preferably; After the heating agent of introducing via the heating agent of heating agent heating unit 15 inlet 151 18 heats in heating agent heating unit 15; After heating agent outlet 152 discharges through heating agent heating unit 15; Blowback heating agent inlet 133 via pressurized raw filtration unit 13 gets in the pressurized raw filtration unit 13, in pressurized raw filtration unit 13, carries out blowback, drying treatment.The gas-oil mixture that to discharge from the gas-oil mixture of pressurized raw filtration unit 13 outlet 134 is incorporated into the gas and oil separating plant 14 via the gas-oil mixture inlet 141 of gas and oil separating plant 14, and this gas-oil mixture separates through gas and oil separating plant 14.Then, the heating agent that makes gained is discharged from the blowback heating agent outlet 143 of gas and oil separating plant 14, is incorporated into the heating agent heating unit 15 from the heating agent inlet 151 of heating agent heating unit 15, supplies to recycle.To be sent in the fractionation by distillation device 9 via the extraction mixture of oil content in second storage tank 8 that the oil content outlet 142 of gas and oil separating plant 14 is discharged, first solvent 2 of recovery and second solvent 19 are discharged with second solvent outlet 95 that reclaims via first solvent outlet 94 of the recovery of fractionation by distillation device 9.First solvent that reclaims is fed in the residue extraction plant 3 through first colvent inlet 35 of the recovery of residue extraction plant 3, supplies to recycle.Second solvent 19 that reclaims is fed in the extraction plant 5 via second colvent inlet 55 of the recovery of extraction plant 5 more again, supplies to recycle.And obtain the extraction product heavy liquefaction oil 16 and high-quality asphalt matter 17 of coal liquefaction residue.。
Wherein, the particle diameter of said coal directly-liquefied residue powder is 0.05～2mm, the ash content of coal 10～30%.
Wherein, said residue extraction plant and again extraction plant be provided with whipping device and recycle pump.
Wherein, said first solvent and second solvent are the liquefaction oil product that directly produces in the DCL/Direct coal liquefaction process.Particularly, first extraction solvent is 160～260 ℃ a fraction, and second extraction solvent is the fraction of IBP～110 ℃.
Wherein, the extracting operation condition of said first solvent is: the mass ratio of coal liquefaction residual powder and said first solvent is 1: 1～10, be preferably 1: 2～and 8; N
2And/or H
2Atmosphere, pressure is 0.1～3.0MPa, is preferably 0.2～2.5MPa; Extraction temperature is 60～300 ℃, is preferably 80～250 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min; The solid concentration of extraction back system is 5～30%, and system density is 0.95～1.5g/ml.
Wherein, said extraction mixture and the solid concentration that extracts the clear liquor phase mixture of the upper strata overflow that mixture obtains again after rotational flow separation are 1%～5%, and the solid concentration of spissated underflow mixture is 40～60%.
Wherein, the condition of extracting operation again of said second solvent is: the mass ratio of coal liquefaction residue and said second solvent is 1: 1～10, be preferably 1: 1～and 6; N
2And/or H
2Atmosphere, pressure is 0.2～3.5MPa, is preferably 0.5～2.5MPa; Extraction temperature is 30～250 ℃, is preferably 40～150 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min.
Wherein, the clear liquor phase mixture of the upper strata overflow of said rotational flow separation acquisition obtains solid concentration and is not more than 0.01% filtrating after secondary filter.
Wherein, the pressure-losses of said cyclone separator is 0.1～1.0MPa.
Wherein, the pore size filter of said secondary filter employing is 0.5～3 μ m.
Wherein, the said spissated underflow mixture that extracts again obtains solid concentration and is not more than 5% filtrating after pressurized raw is filtered.
Wherein, the pore size filter of said pressurized raw filtration employing is 10～50 μ m.
Wherein, the solid concentration of said pressurized raw filtered filtration residue is 70～90%.
Wherein, said secondary filter device and pressurized raw filtration unit are provided with pressure equipment and blowback air system are provided.
Wherein, said heating agent is meant nitrogen, helium rare gas element and water vapor or their mixture, and it is heated to 100～300 ℃ in heating unit, is used for the blowback drying treatment of coarse filtration filter residue.
Wherein, said fractionation by distillation device is air distillation tripping device, underpressure distillation tripping device or both combinations, preferably both combinations.
Another aspect of the present invention provides a kind of by the heavy liquefaction oil and the bitumen that extract according to the method for the invention.
Preferably, be 260～450 ℃ by the boiling range of the heavy liquefaction oil that extracts according to the method for the invention, be particularly suitable for solvent as coal direct liquefaction technology, also be that further unifining becomes other processed oil, like the high quality raw material of diesel oil, solvent oil.
Preferably, less than 0.1%, it is the high quality raw material of preparation carbon materials by the ash of the bitumen that extracts according to the method for the invention.
Provided by the invention a kind of from coal directly-liquefied residue extraction heavy liquefaction oil and bitum method; Its characteristics are; Cyclone separator and filtration unit separation efficiency is high, that be fit to long-term operation are coupled; The solid-liquid separation that is used for liquefied residue extract and extract remainder, the whole process flow process is simple, easy and safe to operate, separation efficiency is high, facility investment is little, be fit to long-term operation.
Provided by the invention a kind of from coal directly-liquefied residue extraction heavy liquefaction oil and bitum method; Its characteristics are; The spissated extraction mixture of eddy flow underflow is extracted with second solvent again, and carry out coarse filtration, hot blowback drying treatment, thereby improve solvent recovering yield extracting the underflow mixture again; Increase the percentage extraction of liquefied residue, thereby improve the economy of extraction process.
Provided by the invention a kind of from coal directly-liquefied residue extraction heavy liquefaction oil and bitum method, its characteristics are that two kinds of extraction solvents are all from the gelatin liquefaction process; For the liquefaction oil product of different fractions section, from the horse's mouth, with low cost; Easy recovery can supply to recycle for a long time.
Provided by the invention a kind of from coal directly-liquefied residue extraction heavy liquefaction oil and bitum method; Its characteristics are, from liquefied residue, extract the heavy liquefaction oil, not only can improve the overall oily yield of gelatin liquefaction process; Avoid the residue wasting of resources, thereby improve the economy of liquefaction factory; And be the coal liquefaction solvent that suits, can improve the degree of heaviness of coal liquefaction solvent, help the gelatin liquefaction reaction.
Provided by the invention a kind of from coal directly-liquefied residue extraction heavy liquefaction oil and bitum method, its characteristics are that the condensation degree of the bitumen aromatic ring that from liquefied residue, extracts is high; The C/H atomic ratio is high; Quinoline insolubles is low, and ash content is low, is the high quality raw material of preparation carbon materials.
Further specify the present invention through the following example, but protection scope of the present invention is not limited to the following example.
Embodiment
The fundamental test flow process is following:
The coal direct liquefaction residue that produces in a kind of 0.1t/d coal direct liquefaction of this experiment selected device, residue character sees attached list 1.At first residue is crushed to below the 2mm with jaw crusher.As shown in Figure 1, coal directly-liquefied residue powder after the 100Kg fragmentation 1 and 300Kg first solvent 2 are joined in the residue extraction plant 3, by carrying out extracting operation under the extraction conditions shown in the subordinate list 2; Extraction have stir and the pump circulation condition under carry out, will extract solidliquid mixture then and be pumped into first cyclone separator 4 and carry out solid-liquid separation, obtain the clear liquor phase mixture 301.5Kg of upper strata overflow; Solid concentration is 2.1%; Flow into first storage tank 6, be pressed into secondary filter device 7 then, the filter pore size is 1 μ m; The solid concentration that obtains filtrating is 0.005%, flows in second storage tank 8.First cyclone separator, 4 bottoms spissated underflow mixture 98.5Kg, solid concentration 47.1% flows in the extraction plant 5 again, adds 200Kg second solvent 19 again, by carrying out extracting operation again under the extraction conditions again shown in the table 2.Extraction have stir and the pump circulation condition under carry out; To extract solidliquid mixture again is pumped into second cyclone separator 12 and carries out solid-liquid separation; Obtain the clear liquor of the extraction again phase mixture 210.1Kg of upper strata overflow, solid concentration is 1.9%, flows into first storage tank 6; After secondary filter device 7 filters, flow into second storage tank 8 then.The spissated underflow mixture 88.4Kg that extracts again in second cyclone separator, 12 bottoms, solid concentration 50.1% is sent into pressurized raw filtration unit 13, carries out the hot pressing coarse filtration.The filter pore size is 50 μ m, and the 25.8Kg that must filtrate again through secondary filter device 7, flows into second storage tank 8.
Heating agent 18 usefulness nitrogen after heating agent heating unit 15 is heated to 150 ℃, carry out blowback, drying treatment to pressurized raw filtration unit 13 as thermal medium; The gas-oil mixture that heating agent carries out is after tripping device 14 separates, and the heating agent that obtains recycles; The extraction mixture of the oil content 18.0Kg that obtains in the tripping device 14 in second storage tank 8 sent in the fractionation by distillation device 9; Reclaim second solvent 19 and first solvent 2 and supply to recycle, and obtain the extraction product heavy liquefaction oil 16 and high-quality asphalt matter 17 of coal liquefaction residue.
The character data of table 1 coal directly-liquefied residue
*Oil content refers to the normal hexane soluble part in the residue in the soxhlet extraction, the bituminous matter insoluble THF soluble part of hexane of making a comment or criticism, and insolubles refers to the insoluble part of THF.
*Comprise asphaltene and preceding asphaltene in the residue.
The main extraction process condition of table 2 embodiment
The experimental result of table 3 coal directly-liquefied residue in the method for the invention
Comparative example
In order to further specify the technique effect of method of the present invention; Comparative example 1 adopts the method for coal directly-liquefied residue same as the previously described embodiments, first extraction solvent, extraction conditions and identical distillating recovering solvent; Adopt conventional hot pressure filtration method to carry out solid-liquid separation, main experimental result is seen table 4.
Comparative example 2 adopts the method for coal directly-liquefied residue same as the previously described embodiments, first extraction solvent, extraction conditions and identical distillating recovering solvent, adopts conventional settling methods to carry out solid-liquid separation, and main experimental result is seen table 4.
Table 4 is according to the experimental result of the coal directly-liquefied residue of traditional method
Data from table 3 and table 4 can be found out; Compare with experimental result according to the coal directly-liquefied residue of traditional method; According to method of the present invention, the percentage extraction of coal directly-liquefied residue, heavy liquefaction oil and bitum yield are high, and the recovery of extraction solvent is high; The continuous long-term operation that helps the residue extraction process, the economy of raising DCL/Direct coal liquefaction technology.
Invention has been described with reference to embodiment and embodiment.Yet, the aspect that the present invention is not limited to describe in the above-described embodiment and examples, and can carry out various distortion.But should be appreciated that for a person skilled in the art, under the situation that does not deviate from the spirit and scope of the present invention, can carry out various modifications and be equal to replacement the present invention.Therefore, the invention is not restricted to the specific embodiment described in this article.More properly, protection scope of the present invention is limited by the accompanying claims.
Claims (19)
1. the method for extraction heavy liquefaction oil and a bitumen from the coal direct liquefaction residue said method comprising the steps of:
A) coal liquefaction residual powder is joined with first solvent carry out thorough mixing extraction in the residue extraction plant, so that comprise heavy liquefaction oil and bitum extractable matter in the liquefied residue are extracted in first solvent;
B) utilize first cyclone separator that comprise first solvent, heavy liquefaction oil, bitum extraction mixture and the residue extract remainder that obtains in the step a) carried out solid-liquid separation, obtain the spissated underflow mixture of clear liquor phase mixture and bottom of upper strata overflow respectively;
C) the spissated underflow mixture in the bottom in the step b) is sent to second solvent again carries out extraction treatment again in the extraction plant, first solvent of carrying secretly in the underflow mixture and extractable matter are extracted in second solvent again, to obtain to extract again mixture;
D) utilize second cyclone separator to comprise first solvent, second solvent, heavy liquefaction oil, bitumly extract mixture again and the residue extract remainder carries out the solid-liquid separation second time, obtain the spissated underflow mixture that extracts again of clear liquor phase mixture of extraction again and bottom of upper strata overflow respectively what obtain in the step c);
E) clear liquor phase mixture in the step b) and the clear liquor of the extraction again phase mixture in the step e) are carried out secondary filter in the secondary filter device, and filtrating is sent in the fractionation by distillation device;
F) the spissated underflow mixture that extracts again in the bottom in the step d) is carried out pressurized raw and filters in the pressurized raw filtration unit, the filtrating part with extract the clear liquor phase mixture again through secondary filter, send into the fractionation by distillation device;
G) in the fractionation by distillation device, the extraction mixture is separated, supply to recycle, and obtain heavy liquefaction oil and ash less than 0.1% bitumen to reclaim first solvent, second solvent.
2. method according to claim 1, wherein, said method also comprises step h between step f) and step g)): remaining filter residue carried out drying treatment with the heating agent blowback after pressurized raw was filtered in to step f), reclaimed residual solvent, sent into the fractionation by distillation device.
3. method according to claim 1; Wherein, Said first solvent and second solvent are in the DCL/Direct coal liquefaction process liquefaction oil product that directly produces, and said first solvent is 160～260 ℃ a fraction, and said second solvent is the fraction of over point (IBP)～110 ℃.
4. method according to claim 1, wherein, the extracting operation condition in said step a) is: the mass ratio of coal liquefaction residue and said first solvent is 1: 1～10, be preferably 1: 2～8; N
2And/or H
2Atmosphere, pressure is 0.1～3.0MPa, is preferably 0.2～2.5MPa; Extraction temperature is 60～300 ℃, is preferably 80～250 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min; The solid concentration of extraction back system is 5～30%, and system density is 0.95～1.5g/ml.
5. method according to claim 1; Wherein, At said step b) and d) in extraction mixture and the solid concentration that extracts the clear liquor phase mixture of the upper strata overflow that mixture obtains again after rotational flow separation be 1%～5%, the solid concentration of the spissated underflow mixture in bottom is 40～60%.
6. method according to claim 1, wherein, the condition of extracting operation again of second solvent is in said step c): the mass ratio of coal liquefaction residue and said second solvent is 1: 1～10, be preferably 1: 1～6; N
2And/or H
2Atmosphere, pressure is 0.2～3.5MPa, is preferably 0.5～2.5MPa; Extraction temperature is 30～250 ℃, is preferably 40～150 ℃; The extraction time is 5～120min, and stir speed (S.S.) is 50～400r/min.
7. method according to claim 1, wherein, the clear liquor phase mixture of the upper strata overflow that rotational flow separation obtains in said step e) obtains solid concentration and is not more than 0.01% filtrating after secondary filter.
8. method according to claim 1, wherein, the pore size filter of the secondary filter device that in said step e), uses is 0.5～3 μ m.
9. method according to claim 1, wherein, the spissated underflow mixture that extracts again obtains solid concentration and is not more than 5% filtrating after pressurized raw is filtered in said step f).
10. method according to claim 1, wherein, the pore size filter of the pressurized raw filtration unit that in said step f), uses is 10～50 μ m.
11. method according to claim 1, wherein, the solid concentration of pressurized raw filtered filtration residue is 70～90% in said step f).
12. method according to claim 2; Wherein, At said step h) in heating agent be meant nitrogen, helium rare gas element and water vapor or their mixture, said heating agent is heated to 100～300 ℃ in heating unit, be used for the blowback drying treatment of coarse filtration filter residue.
13. method according to claim 2, wherein, at said step h) in, reclaim residual solvent and at least one oil-gas separator, carry out.
14. method according to claim 1, wherein, in said step g), said fractionation by distillation device is atmospheric distillation tower, vacuum still or both combinations, preferably both combinations.
15. method according to claim 1, wherein, the particle diameter of said coal directly-liquefied residue powder is 0.05～2mm.
16. method according to claim 1, wherein, said residue extraction plant and again extraction plant be provided with whipping device and recycle pump.
17. method according to claim 1, wherein, said secondary filter device and pressurized raw filtration unit are provided with pressure equipment and blowback air system are provided.
18. one kind by the heavy liquefaction oil and the bitumen that extract according to each described method among the claim 1-17.
19. heavy liquefaction oil according to claim 18 and bitumen, wherein, the boiling range of said heavy liquefaction oil is 260～450 ℃, and the ash of said bitumen is less than 0.1%.
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