CN202246572U - System for treating coal direct liquefied residue - Google Patents

System for treating coal direct liquefied residue Download PDF

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Publication number
CN202246572U
CN202246572U CN2011203713568U CN201120371356U CN202246572U CN 202246572 U CN202246572 U CN 202246572U CN 2011203713568 U CN2011203713568 U CN 2011203713568U CN 201120371356 U CN201120371356 U CN 201120371356U CN 202246572 U CN202246572 U CN 202246572U
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China
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little
outlet
coal
residue
coal liquefaction
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CN2011203713568U
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李志明
李克健
杨强
张胜振
汪华林
吴秀章
吕文杰
章序文
王剑刚
李永伦
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East China University of Science and Technology
China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Group Corp Ltd
Shanghai Research Institute of China Shenhua Coal to Liquid Chemical Co Ltd
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East China University of Science and Technology
China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Group Corp Ltd
Shanghai Research Institute of China Shenhua Coal to Liquid Chemical Co Ltd
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Abstract

The utility model relates to a system for treating coal direct liquefied residue, which comprises a (A) mixer, (B) a micro-hydrocyclone separation unit, (C) a filter and (D) a precise filter, wherein the mixer is at least provided with an extraction solvent inlet, a coal direct liquefied residue inlet and a coal liquefied residue extraction mixture outlet; the micro-hydrocyclone separation unit is at least provided with a coal liquefied residue extraction mixture inlet connected with the coal liquefied residue extraction mixture outlet, a concentrated coal liquefied coal residue bottom flow outlet and a clean liquid phase mixture outlet; the filter is at least provided with a concentrated coal liquefied residue bottom flow inlet connected with the concentrated coal liquefied residue bottom flow outlet and a filter liquid outlet; and the precise filter is at least provided with a clean liquid phase mixture inlet connected with the clean liquid phase mixture outlet, a precise filtration clean filtrate outlet and a precise filtration intercept phase outlet. The system for treating the coal direct liquefied residue has high reliability and separation efficiency.

Description

A kind of system that handles coal directly-liquefied residue
Technical field
The utility model relates to a kind of treatment system of coal directly-liquefied residue, particularly relates to a kind of to carry out the system of solid-liquid separation through the coal directly-liquefied residue after fully extracting.Specifically, the utility model provides a kind of little cyclone separator and solvent extraction process coupling and intensifying to handle the system of coal directly-liquefied residue.
Background technology
Technology of direct coal liquefaction is the coal generation pyrolysis that under high temperature, high pressure, makes in the high density coal slurry, under catalyst action, carries out hydrogenation and further decomposes, and changes into the liquid fuel (petroleum naphtha, diesel oil etc.) of cleaning or the advanced clean coal technology of industrial chemicals.DCL/Direct coal liquefaction technology can be divided into three formants.1. coal slurry prepares the unit: coal is crushed to<below the 0.2mm, process coal oil mixture (or title " coal paste ") with solvent, catalyzer.2. gelatin liquefaction reaction member: the coal in the coal slurry (is generally direct hydrogenation 17~30MPa) times, coal is changed into liquid product at high temperature (about 450 ℃), high pressure.3. product separating unit: will react the gas, the product liquid that generate and separate (mainly comprise solution-air is separated, solid-liquid separate) with residue.
Coal also has some solidss behind hydrogenation liquefaction, they mainly are inert fractions in inorganic mineral in the coal, catalyzer and the unconverted coal.At the product separating unit, through solid-liquid separation process solids and liquefaction oil are being separated usually, the solids of gained is referred to as residue.The liquefied residue that gelatin liquefaction factory produces is a kind of high-carbon, high ash and doctor positive material; The different material coal is different with the residue characteristic that different liquefaction process produce; In some technology, can account for about 30% of liquefaction feed coal total amount; No matter adopt which kind of technology, all can carry a part of heavy liquefaction oil in the residue secretly simultaneously.The separation of liquefied residue with utilize the integrity directly influence liquefaction process and the cost that liquefies, be one of coal high-efficiency direct liquefaction technology key technical problem that must solve.
The solid-liquid separation of coal liquefaction residue has following difficult point: the solid particulate granularity is very thin, and size-grade distribution partly is suspended in the raffinate from less than 1 micron to several microns, and part is colloidal state; The existence of preceding asphaltene and glutinous thing such as height such as asphaltene grade, and unconverted coal swelling and precipitation-peptization therein all can make viscosity very high; Two alternate density differences are very little.Up to the present, the solid-liquid separation technique that is adopted mainly contains filter method, gravity settling separation method, eddy flow centrifugal settling separation method, distillation separation method, anti-solvent method, critical solvent deliming of hot suction filtration mode of vacuum and pressurized heat filter type etc.Wherein, vacuum flashing (or underpressure distillation) law technology is ripe, with basically not the distilled oil of asphaltenes-containibinders be turning oil, viscosity of coal slurry is low, the hydrogenation reaction performance improves; The thick oil of liquefaction that the employing underpressure distillation is carried out after the solid-liquid separation does not generally contain ash; While alternative up to a hundred centrifugal filters of flashing tower, treatment capacity heightens, and does not need loaded down with trivial details filter operation, and equipment and operation are all greatly simplified.Just because of these advantages, this technology has obtained using widely, and German novel process, U.S. SRC-II, H-Coal, EDS and Chinese Shenhua all adopt should technology.But; For making the residue that stays keep certain fluidity, so that pumping can not let oil all gasify; Make and contain the have an appointment thick oil of a certain amount of liquefaction and asphaltene and preceding asphaltene in the residue in the liquefied residue; Solids content is controlled at below 50%, and about 160 ℃ of softening temperature makes the total recovery that has reduced product liquid.
Aspect residue utilized, the residue in the research and development utilized approach to mainly contain solvent extraction, destructive distillation (coking), the raw material as gasification hydrogen-producing, burning and non-burning utilization.Resource is not only wasted in burning, also contaminate environment.The content of materials such as the asphaltene class in the liquefied residue is about about 20% of level of residue; Mainly form by the polycyclic condensed aromatics; Have the aromaticity height, carbon content is high, easily polymerization or crosslinked characteristics; Being suitable as very much the raw material of preparation carbon materials, is a kind of very valuable and unique resource.Chinese patent ZL200510047800.X discloses a kind of method for preparing nano-carbon material with the coal direct liquefaction residue as the raw material plasma body.Chinese patent ZL200610012547.9 discloses a kind of with the method for coal liquefaction residue as road asphalt modifier.Chinese patent CN101591819 discloses a kind of method of utilizing coal directly-liquefied residue to prepare asphalt base carbon fiber.Chinese patent CN101580729 discloses a kind of method for preparing mesophase pitch with coal liquefaction residue.These methods all are that the bitumen with coal liquefaction residue is a raw material, do not relate to the utilization of the heavy oil content in the residue organic matter, and the extracting of residue medium pitch class material all is to be solvent with expensive pure chemistry reagent, and cost is higher relatively.Heat treating methods such as common destructive distillation, coking can be realized the purpose of separating, reclaim the heavy liquefaction oil of BO and pitch coke.ZL201020003508.4 discloses a kind of continuous coking equipment of coal liquefied residue.CN101760220A discloses a kind of method for continuously coking and equipment of coal liquefied residue.But because aromaticity content is high in the heavy liquefaction oil, the aromatic hydrocarbons condensation degree is high, and violent polycondensation reflection will take place in heat treatment process, and the heavy oil content polycondensation of significant proportion is a coke, and therefore the ratio of the actual heavy oil product that obtains is not high.Be difficult to reach the purpose of utilizing gelatin liquefaction heavy liquefaction oil fully, rationally, efficiently.The method of liquefied residue being carried out gasification hydrogen-producing is a kind of approach that effectively utilizes on a large scale; But the high value added utilization potentiality to bitumen in the residue and BO do not obtain embodying; And ash content is up to more than 20% in the residue, and this brings very big influence will for the deslagging of vapourizing furnace.
Chinese patent CN101962560A discloses a kind of application of extracting process and extract of coal directly-liquefied residue; With the liquefaction oil product that directly produces in the DCL/Direct coal liquefaction process as extraction solvent; Behind appropriate hydrogenation, use the heavy oil product in the coal liquefaction residue, substitute the light component in the former circulating solvent, not only can increase the yield of liquefaction oil product as circulating solvent; And this heavy solvent performance is better, and technology is simple.This method has realized separating of the thick oil of liquefaction, bitumen and solid residue simultaneously, has farthest brought into play the potentiality of utilizing of coal liquefaction residue.Chinese patent CN101962561A is the same basically with the CN101962560A thinking; Liquefied residue is carried out solvent extraction earlier; Carry out solid-liquid and liquid-liquid separation again, just extract route difference to some extent, but all do not provide the concrete scheme of extraction mixture solid-liquid separation.
It is thus clear that; The development trend of gelatin liquefaction product solid-liquid separation process does at present; Utilize the solid-liquid separation process of vacuum flashing (underpressure distillation) to obtain the solid phase weight concentration, utilize the DCL/Direct coal liquefaction oil product to carry out extracting again, again solvent extractable matter is carried out solid-liquid and liquid-liquid separation as solvent less than 50% coal liquefaction residue; Realize that the thick oil of liquefaction, bitumen separate with the maximization of solid phase residue in the coal liquefaction residue, and sufficient recycling.Yet; At present also seldom to the separate study of solid-liquid system behind the solvent extraction; Chinese patent CN101962561A and CN101962560A mention slightly; Mainly be engaged in the U.S. Kerr-MCGEE company of solid separate study in the various gelatin liquefaction products and the ITSL process using gravitational settler of Lummus and separate this system, efficient is relatively low.This system stalling characteristic is similar with the solid-liquid system that carries out vacuum flashing (underpressure distillation), separates relatively difficulty, and traditional methods such as strainer, whizzer have complicated operation; Cost is high; Shortcomings such as safety is low, separation efficiency need improve as far as possible here simultaneously, also is not suitable for using flash method again.
Therefore, it is low that this field presses for the development investment cost, and safety is high, and cycle of operation is long, and the high solvent residue separation system of separation efficiency.
The utility model content
The utility model relates to a kind of system that handles coal directly-liquefied residue, comprising:
(A) mixing tank has extraction solvent inlet, coal directly-liquefied residue inlet and coal liquefaction residue extraction mixture outlet at least;
(B) little omitted has at least
Coal liquefaction residue extraction mixture inlet, wherein, coal liquefaction residue extraction mixture outlet is connected to coal liquefaction residue extraction mixture inlet,
Concentrate the outlet of coal liquefaction residue underflow, and
The outlet of clear liquor phase mixture;
(C) strainer has at least
Concentrate the import of coal liquefaction residue underflow, be connected to and concentrate the outlet of coal liquefaction residue underflow,
Filtrate outlet; And
(D) accurate filter has at least
Clear liquor phase mixture inlet is connected to the outlet of clear liquor phase mixture,
The outlet of secondary filter clear filtrate, and
Outlet is mutually held back in secondary filter.
Preferably, (C) filtrate outlet of strainer and/or secondary filter are held back mutually outlet and are connected to (A) mixing tank.
Preferably, this system further comprises: (E) storage tank, (C) filtrate outlet of strainer and/or secondary filter are held back (E) storage tank of outlet process mutually and are connected to (A) mixing tank.
Preferably, (B) little omitted comprises one or more little cyclone separators, and each little cyclone separator all has little cyclone separator inlet, little eddy flow concentrates underflow outlet and the outlet of clear liquor phase mixture.
Preferably, (B) little omitted is multistage little omitted.
Preferably, wherein, the little cyclone separator inlet of the first step is as coal liquefaction residue extraction mixture inlet; The little eddy flow of the first step concentrates the underflow outlet as concentrating the outlet of coal liquefaction residue underflow;
Wherein, the outlet of the clear liquor phase mixture of the little cyclone separator of last step is as the clear liquor phase mixture outlet of little omitted;
Wherein, the outlet of the underflow of little cyclone separator is connected to (A) mixing tank more than the second stage;
Wherein, the outlet of the clear liquor phase mixture of other each the little cyclone separator except that the little cyclone separator of last step is connected to the little cyclone separator inlet of next stage.
Preferably, (B) little omitted is the little omitted of two-stage.
Preferably, the outlet of the underflow of little cyclone separator is connected to (A) mixing tank more than the second stage.
Preferably, (B) the concentrated coal liquefaction residue underflow of little omitted exports the concentrated coal liquefaction residue underflow import that is connected to (C) strainer via (F) helix transporting device.
Preferably, (E) storage tank is connected to (A) mixing tank via transh pump.
Preferably, coal liquefaction residue extraction mixture outlet is positioned at the bottom of (A) mixing tank, and is connected to the top of (A) mixing tank.
Preferably, the little cyclone separator of each grade all is many little rotational flow separation core pipe parallel connections.
This system reliability is high, and separation efficiency is high.
Description of drawings
Fig. 1 is the schematic flow sheet according to an embodiment of the utility model.
Fig. 2 is the schematic flow sheet according to another embodiment of the utility model.
Embodiment
In the utility model, under the situation of not contradiction or conflict, all embodiment, embodiment and the characteristic of the utility model can make up each other.
In the utility model, all units, parts etc. both can be purchased, also can be according to the disclosed content self-control of the utility model.
In the utility model, for the emphasis of outstanding the utility model, the omission that some conventional operations and unit, parts are carried out, or only do simple description.
In the utility model, " with ... link to each other " or " being connected to " or " connections ", both can be that the two directly links to each other, also can across common parts or device (for example valve, pump, interchanger etc.) links to each other or connection.
In the utility model, " coal directly-liquefied residue " and " coal liquefaction residue " interchangeable use all refers to the coal liquefaction residue that the solid-liquid separation process of gelatin liquefaction product utilization vacuum flashing (underpressure distillation) obtains.
The contriver of the utility model finds through after the extensive and deep research; The development trend of gelatin liquefaction product solid-liquid separation process does at present; Utilize the solid-liquid separation process of vacuum flashing (underpressure distillation) to obtain the solid phase weight concentration less than 50% coal liquefaction residue; Utilize the DCL/Direct coal liquefaction oil product to carry out extracting again as solvent; Again solvent extractable matter is carried out solid-liquid and liquid-liquid separation, realize that the thick oil of liquefaction, bitumen separate with the maximization of solid phase residue in the coal liquefaction residue, and sufficient recycling.In this route; The solid-liquid separation that coal directly-liquefied residue is carried out behind the solvent extraction is the committed step that is related to this technology whole separation effect and running cost; Present domestic also do not have relevant patent and bibliographical information; Shortcomings such as traditional strainer, whizzer have complicated operation, and cost is high, and safety is low.Simultaneously, the contriver finds that also cyclone separator has that volume is little, cost is low, and processing speed is fast; Movement-less part; Flexibility is strong, and is simple to operate, the advantage that safety is high; With the pre-treatment of rotational flow separation, can improve the separation and the processing property of strainer, whizzer greatly simultaneously as strainer, whizzer.Based on above-mentioned discovery, make full use of the advantage of cyclone separator, the utility model is accomplished.
The utility model adapts to the developing direction of coal directly-liquefied residue treatment technology; Make full use of having a few that rotational flow separation is simple in structure, cost is low, safety is high; Combine with solvent extraction process, a kind of method of efficient solid-liquid separation and system of this method of realization that coal directly-liquefied residue is carried out is provided.
The system that relates in one aspect to the processing coal directly-liquefied residue of the utility model comprises:
(A) mixing tank has extraction solvent inlet, coal directly-liquefied residue inlet and coal liquefaction residue extraction mixture outlet at least;
(B) little omitted has at least
Coal liquefaction residue extraction mixture inlet is connected to coal liquefaction residue extraction mixture outlet,
Concentrate the outlet of coal liquefaction residue underflow, and
The outlet of clear liquor phase mixture;
(C) strainer has at least
Concentrate the import of coal liquefaction residue underflow, be connected to and concentrate the outlet of coal liquefaction residue underflow,
Filtrate outlet; And
Optional (D) accurate filter has at least
Clear liquor phase mixture inlet is connected to the outlet of clear liquor phase mixture,
The outlet of secondary filter clear filtrate, and
Outlet is mutually held back in secondary filter.
Preferably, (C) filtrate outlet of strainer and/or secondary filter are held back mutually outlet and are connected to (A) mixing tank.
Preferably, the system of the utility model further comprises: (E) storage tank, (C) filtrate outlet of strainer and/or secondary filter are held back (E) storage tank of outlet process mutually and are connected to (A) mixing tank.Preferably, (E) storage tank is connected to (A) mixing tank via transh pump.
(E) storage tank has liquid-inlet and liquid exit at least.
Preferably, (C) filtrate outlet of strainer and/or secondary filter are held back the storage tank of outlet process mutually and are connected to (A) mixing tank.(C) filtrate outlet of strainer and/or secondary filter are held back the liquid exit that exports the liquid-inlet storage tank that is connected to storage tank mutually and are connected to (A) mixing tank.
For example, (E) storage tank can be the various forms of storage tanks that can store returning charge, tower etc.
Preferably, coal liquefaction residue extraction mixture outlet is positioned at the bottom of (A) mixing tank.Coal liquefaction residue extraction mixture outlet also is connected to the top of (A) mixing tank, thereby makes a coal liquefaction residue extraction mixture part get into (B) little omitted, and another part returns (A) mixing tank.
Preferably, (A) mixing tank has the recycle stock inlet, is positioned at the top or the top of (A) mixing tank.In one embodiment, coal liquefaction residue extraction mixture outlet also is connected to the recycle stock inlet of (A) mixing tank.
(B) little omitted can comprise one or more little cyclone separators.Each little cyclone separator has: little cyclone separator inlet, little eddy flow concentrates the underflow outlet, and the outlet of clear liquor phase mixture.
(B) little omitted can be one or more levels little omitted (little omitted more than the two-stage).When little omitted was multistage little omitted, little omitted can comprise placed in-line a plurality of little cyclone separator.For example, when little omitted was the little omitted of two-stage, little omitted comprised: the little cyclone separator of the first step, the little cyclone separator in the second stage.By that analogy, multistage little omitted can comprise: the little cyclone separator of the first step, and the little cyclone separator in the second stage ...., the little cyclone separator of n level.For example, n >=2; N >=3 for example also are like n >=4 or n >=5.Consider and simplify technology and net effect, preferred little omitted is the little omitted of two-stage, and promptly little omitted is made up of the little cyclone separator of two-stage.
When little omitted was multistage little omitted, the little rotational flow separation of the first step obtained concentrating coal liquefaction residue underflow (being that the little eddy flow of the first step concentrates underflow) and the little cyclone clarification liquid of the first step.When little omitted was multistage little omitted, the little cyclone separator inlet of the first step was as coal liquefaction residue extraction mixture inlet; The little eddy flow of the first step concentrates the underflow outlet as concentrating the outlet of coal liquefaction residue underflow.
When adopting multistage little omitted, the clear liquor phase mixture outlet of the little cyclone separator of last step is as the clear liquor phase mixture outlet of little omitted.
Preferably, when adopting multistage little omitted, the outlet of the underflow of little cyclone separator is connected to (A) mixing tank more than the second stage.Preferably, the outlet of the underflow of little cyclone separator is connected to (A) mixing tank through storage tank more than the second stage.The outlet of the underflow of little cyclone separator is connected to the liquid-inlet of storage tank more than the second stage, and the liquid exit of storage tank is connected to (A) mixing tank.
Preferably, when adopting multistage little omitted, the clear liquor phase mixture outlet of other each the little cyclone separator except that the little cyclone separator of last step is connected to the little cyclone separator of next stage and enters the mouth.
Preferably, little omitted is the little omitted of two-stage, comprising:
(B1) the little cyclone separator of the first step comprises:
The little cyclone separator inlet of the first step as coal liquefaction residue extraction mixture inlet, is connected to coal liquefaction residue extraction mixture outlet,
The little eddy flow of the first step concentrates the underflow outlet, as concentrated coal liquefaction residue underflow outlet, is connected to the concentrated coal liquefaction residue underflow import of strainer, and
The outlet of first step clear liquor phase mixture;
(B2) the little cyclone separator in the second stage comprises:
The little cyclone separator inlet in the second stage links to each other with the outlet of first step clear liquor phase mixture,
The little eddy flow in the second stage concentrates the underflow outlet,
The little cyclone clarification liquid outlet in the second stage, the clear liquor phase mixture that is connected to accurate filter enters the mouth.
Preferably, the little eddy flow in the second stage concentrates the underflow outlet and is connected to (A) mixing tank.Preferably, the outlet of the underflow of the little cyclone separator in the second stage is connected to (A) mixing tank through storage tank.The underflow outlet of the little cyclone separator in the second stage is connected to the liquid-inlet of storage tank, and the liquid exit of storage tank is connected to (A) mixing tank.
Preferably, (B) the concentrated coal liquefaction residue underflow of little omitted exports the concentrated coal liquefaction residue underflow import that is connected to (C) strainer via (F) transmitting device.
(A) mixing tank can be stirring tank, various forms of reaction kettles, storage tank, tower and pipeline etc. with mixing functions.
(C) strainer can be pressure filter, leaf filter, vacuum filtration machine, centrifugal filter, cross-flow filter, film filter etc.
(D) accurate filter can be can separating low concentration the pressure filter, leaf filter, vacuum filtration machine, centrifugal filter, cross-flow filter, film filter etc. of fine particle.
(F) transmitting device can be worm conveyor, endless belt conveyor, buried scraper transfer roller etc., preferred worm conveyor.
A kind of preferred embodiment in, the utility model provides a kind of little rotational flow separation and solvent extraction process coupling and intensifying to handle the system of coal directly-liquefied residue, this system comprises:
Be used for stirring tank with coal directly-liquefied residue and extraction solvent thorough mixing and extraction; Be connected with stirring tank, be used for the little cyclone separator of the first step of coal liquefaction residue extraction mixture initial gross separation; Be connected with the little cyclone separator of the first step, be used to carry the little eddy flow of the first step to concentrate the worm conveyor of coal liquefaction residue underflow; Be connected with worm conveyor, be used for the pressure filter of gelatin liquefaction solid residue height enrichment; And
Be connected with the little cyclone separator of the first step, be used for the little cyclone separator in the further clarifying second stage of the little cyclone clarification liquid phase mixture of the first step; Be connected with the little cyclone separator in the second stage, be used for the clarifying accurate filter of coal liquefaction residue extraction liquid phase mixture height; And
With the little cyclone separator in the second stage, accurate filter, pressure filter connects, and is used for the topping-up pump of stable storage tank of mass flow and foldback stirring tank.
One preferred embodiment in, the little cyclone separator of each grade can be many little rotational flow separation core pipes parallel connections, satisfies the requirement of treatment capacity.
Another preferred embodiment in, stirring tank, each little cyclone separator, worm conveyor, pressure filter, accurate filter and connecting tube all have 100~200 ℃ measure of insulation.
Another preferred embodiment in, the mounting means of little cyclone separator is vertical.For example, the perhaps slight inclination that the mounting means of little cyclone separator can be vertical.
Another preferred embodiment in, the pressure-losses of little cyclone separator is 0.1~0.4MPa.
Another preferred embodiment in, topping-up pump adopts the special transh pump of carrying solid-liquid two-phase flow, supercharging 0.1~1.2MPa.
An aspect of the utility model relates to the method for utilizing said system to handle coal directly-liquefied residue, and this method comprises:
(a) coal directly-liquefied residue is mixed in mixing tank with extraction solvent, thick oil of the liquefaction in the liquefied residue and bitumen are extracted in the solvent, obtain coal liquefaction residue extraction mixture;
(b) all or part of carries out little rotational flow separation to coal liquefaction residue extraction mixture, obtains concentrating coal liquefaction residue and clear liquor phase mixture;
(c) the concentrated coal liquefaction residue that little rotational flow separation is obtained filters, and obtains filtrating and filter cake;
(e) alternatively, the clear liquor phase mixture is carried out secondary filter, obtain the secondary filter clear filtrate and hold back mutually with secondary filter.
A kind of preferred embodiment in, the utility model provides a kind of little rotational flow separation and solvent extraction process coupling and intensifying to handle the method for coal directly-liquefied residue, this method comprises:
(a), thick oil of the liquefaction in the liquefied residue and bitumen are extracted in the solvent with coal directly-liquefied residue and extraction solvent thorough mixing in mixing tank (for example stirring tank);
(b) coal liquefaction residue extraction mixture is carried out all (or part) little rotational flow separation, realize the initial gross separation of solid residue and liquid phase mixture; And
(c) concentrated coal liquefaction residue underflow helical feed to the pressure filter entrance pressure filter that the little rotational flow separation of the first step is obtained is held back filter cake and is supplied flow to use;
(d) liquid phase mixture through the little cyclone clarification of the first step is carried out the little rotational flow separation in the second stage, obtain further clear liquor phase mixture; And
(e) alternatively, the further clear liquor phase mixture through the little rotational flow separation in the second stage is carried out secondary filter, clear filtrate supplies flow to use;
(f) alternatively, the concentrated underflow of the little eddy flow in the second stage, secondary filter are held back mutually and the mixing of press filtration filtrating, turn back to mixing tank (for example stirring tank), carry out cycling extraction.
In step (a); Extraction solvent can be benzene,toluene,xylene, naphthalene series aromatics, furfural, THF, quinoline, pyridine, N; A kind of or its mixture of at least two kinds in dinethylformamide, DMAC N,N, the N-Methyl pyrrolidone.
A kind of preferred embodiment in, the part of coal liquefaction residue extraction mixture is carried out little rotational flow separation, another part returns mixing tank.
Preferably, in step (b), little rotational flow separation can be one or more levels little rotational flow separation (little rotational flow separation more than the two-stage), the for example little rotational flow separation of two-stage, three grades of little rotational flow separation or the little rotational flow separation of level Four, the preferred little rotational flow separation of secondary.
One preferred embodiment in; Little rotational flow separation can be that one or more levels little rotational flow separation is formed; Improve the concentrated effect of solid phase residue and the clarifying effect of liquid phase mixture respectively as much as possible, also be suitable for handling in other DCL/Direct coal liquefaction technology through the solvent residue solid-liquid system after the extraction.
When adopting multistage little rotational flow separation, the liquid phase mixture (abbreviating " first step clear liquor " as) of concentrated coal liquefaction residue that the little rotational flow separation of the first step obtains (being that the little eddy flow of the first step concentrates underflow) and the little cyclone clarification of the first step.
When adopting multistage little rotational flow separation, first step clear liquor carries out the little rotational flow separation in the second stage, obtains the liquid phase mixture (abbreviating " second stage clear liquor " as) and the concentrated underflow of the little eddy flow in the second stage of the little cyclone clarification in the second stage.By that analogy, carry out little step by step rotational flow separation.Multistage little omitted can comprise: the little rotational flow separation of the first step, and the little rotational flow separation in the second stage ...., the little rotational flow separation of n level.For example, n >=2; N >=3 for example also are like n >=4 or n >=5.Consider and simplify technology and net effect, preferred little rotational flow separation is the little rotational flow separation of two-stage, and promptly little omitted is made up of the little rotational flow separation of two-stage.
When little rotational flow separation was multistage little rotational flow separation, coal liquefaction residue extraction mixture got into the little rotational flow separation of the first step; The little eddy flow of the first step concentrates underflow as concentrating coal liquefaction residue.
Preferably, when little rotational flow separation was multistage little rotational flow separation, the clear liquor phase mixture that the little rotational flow separation of last step obtains carried out secondary filter, obtains the secondary filter clear filtrate and holds back mutually with secondary filter.In step (b); When multistage little rotational flow separation is the little rotational flow separation of two-stage (little rotational flow separation is made up of the little rotational flow separation of two-stage); The clear liquor phase mixture that the little rotational flow separation in the second stage obtains carries out secondary filter, obtains the secondary filter clear filtrate and holds back mutually with secondary filter.
Preferably, when adopting multistage little rotational flow separation, the little rotational flow separation of clear liquor phase mixture entering next stage of other each the little rotational flow separation except that the little rotational flow separation of last step.
Preferably, when little rotational flow separation was multistage little rotational flow separation, little eddy flow that the above little rotational flow separation in the second stage obtains concentrated a underflow part or all turns back to mixing tank (for example stirring tank), carries out cycling extraction.Preferably, little eddy flow that the above little rotational flow separation in the second stage obtains concentrates underflow through the storage tank regime flow, returns mixing tank in the step (a) again as extraction solvent, carries out cycling extraction.
Preferably; When little rotational flow separation is multistage little rotational flow separation; Little eddy flow that the above little rotational flow separation in the second stage obtains concentrates underflow, secondary filter is held back the part in the filtrating in phase, the step (c) or all turned back to mixing tank (for example stirring tank), carries out cycling extraction.
Preferably; Little eddy flow that little rotational flow separation more than the second stage is obtained concentrates underflow, the filtrating mixing in phase, the step (c) is held back in secondary filter; Obtain reclaiming mixed solution, reclaim mixed solution at least a portion, preferably all turn back to mixing tank (for example stirring tank), carry out cycling extraction.For example, little eddy flow that the little rotational flow separation more than the second stage is obtained concentrates underflow, the filtrating process storage tank regime flow in phase, the step (c) is held back in secondary filter, turning back to mixing tank (for example stirring tank), carries out cycling extraction.
Preferably, in step (c), be filtered into press filtration.Filtering (press filtration) can carry out in pressure filter.Preferably, the conveying of concentrated coal liquefaction residue is a helical feed.Preferably, in step (c), filter the filter cake that obtains and supply with the flow use.
Preferably, secondary filter can be carried out through pressurization secondary filter, filter element filtering, barrel type filtering, membrane filtration etc.
Preferably, secondary filter is held back the mixing tank that returns mutually in the step (a) as extraction solvent.
Preferably, the filtrating in the step (c) is returned mixing tank in the step (a) mutually as extraction solvent.
Preferably, the solid phase weight concentration is 10%~60% in the coal liquefaction residue raw material, and is preferred 20%~60%, more preferably 30%~60%, most preferably 30%~55%.
Preferably, coal liquefaction residue and extraction solvent are pressed 1: 1~8 mixed entering mixing tank (for example stirring tank), preferred 1: 1~6, more preferably 1: 1~5, most preferably 1: 1~4.
Preferably, the solid phase true density is 1000~2500kg/m in the coal liquefaction residue extraction mixture 3, preferred 1200~2500kg/m 3, more preferably 1500~2500kg/m 3, 1500~2000kg/m most preferably 3
Preferably, the solid phase weight concentration is 5%~30% in the coal liquefaction residue extraction mixture, and is preferred 10%~30%, more preferably 10%~30%, most preferably 15%~25%.
Preferably, in the coal liquefaction residue extraction mixture particle diameter of solid phase be 32~400 orders (0.038~0.50mm), preferred 0.038~0.20mm, more preferably 0.038~0.10mm, most preferably 0.038~0.05mm.
Another preferred embodiment in; Coal liquefaction residue extraction mixture is through the little rotational flow separation of the first step, obtains the solid phase weight concentration and be 30%~65% concentrated coal liquefaction residue underflow and solid phase weight concentration and be the liquid phase mixture of 0.5%~5% the little cyclone clarification of the first step.
Another preferred embodiment in, it is 0.01%~1.0% further clear liquor phase mixture that the liquid phase mixture of the little cyclone clarification of the first step obtains the solid phase weight concentration through the little rotational flow separation in the second stage.
Another preferred embodiment in, the further clear liquor phase mixture that the little rotational flow separation in the second stage is obtained carries out secondary filter, obtains the solid phase weight concentration and is not more than 0.001% height clear filtrate.
Another preferred embodiment in, it is 80%~95% the filter cake of holding back through obtaining the solid phase weight concentration after the press filtration that helical feed concentrates the coal liquefaction residue underflow to the little eddy flow of the first step of pressure filter.
Below in conjunction with the content of the further sets forth in detail the utility model of embodiment, but these instances do not limit the protection domain of the utility model.
Followingly the utility model is carried out more concrete description with reference to accompanying drawing.
Fig. 1 is the schematic flow sheet according to little rotational flow separation of an embodiment of the utility model and solvent extraction process coupling and intensifying processing coal directly-liquefied residue.
Coal directly-liquefied residue raw material solid phase weight content is 10%~60%.As extraction solvent, in 1 li thorough mixing of mixing tank (for example stirring tank), extraction, obtaining the solid phase weight concentration is 5%~30% coal directly-liquefied residue extraction mixture with coal liquefaction residue and solvent with the DCL/Direct coal liquefaction oil product; Whole tangentials get into the little cyclone separator 2 of the first step to coal liquefaction residue extraction mixture under the pressure of 0.1MPa being not less than, and obtain the solid phase weight concentration and be 30%~65% concentrated coal liquefaction residue underflow and solid phase weight concentration and be 0.5%~5% the little cyclone clarification liquid phase mixture of the first step; The little cyclone clarification liquid phase mixture of the first step gets into the little cyclone separator 3 in the second stage, obtains further clarifying liquid phase mixture, and the solid phase weight content is 0.01%~1.0%; The liquid phase mixture of the little cyclone clarification in the second stage gets into accurate filter 4 again, realizes the height clarification of liquid phase mixture, and clear filtrate changes flow again over to and uses; The concentrated coal liquefaction residue underflow that the little eddy flow of the first step obtains is delivered to pressure filter 6 through worm conveyor 5, realizes that the height of gelatin liquefaction solid residue concentrates, and the solid phase weight concentration is 80%~95%; The little eddy flow in the second stage is concentrated underflow, and secondary filter is held back mutually and press filtration filtrating process storage tank 7 regime flows, turns back to mixing tank (for example stirring tank) 1 through impurity impeller pump 8 again, carries out cycling extraction.
Fig. 2 is the schematic flow sheet according to little rotational flow separation of another embodiment of the utility model and solvent extraction process coupling and intensifying processing coal directly-liquefied residue.This embodiment is the same basically with Fig. 1, and the mixture after just coal directly-liquefied residue extracts through mixing tank (for example stirring tank) 1 partly gets into the little cyclone separator 2 of the first step.
Mixture after coal directly-liquefied residue extracts through mixing tank (for example stirring tank) 1 partly gets into the preswirl separator, can regulate the operating mode that cyclone separator is in stability and high efficiency, can improve separation efficiency than less energy-consumption.So Fig. 2 is optimum flow process.
The major advantage of the utility model is: the utility model method has made full use of cyclone separator compact construction, simple; Cost of investment is low, and is easy to operate, the advantage that safety is high; With the pre-treatment of rotational flow separation as press filtration and secondary filter; Improved the separation and the processing property of strainer greatly, realized that the thick oil of liquefaction, bitumen separate with the maximization of solid phase residue in the coal liquefaction residue, be convenient to follow-up making full use of this resource.
All documents in the utility model topic note are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition after having read the above-mentioned teachings of the utility model, those skilled in the art can do various changes or modification to the utility model, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Certainly, the utility model also can have other embodiments, and the preferred implementation that the above is merely the utility model is not the protection domain that is used for limiting the utility model; Under the situation that does not deviate from the utility model spirit, those of ordinary skills are every to make various corresponding variations and modification according to the utility model content, all belongs to the protection domain of the claim of the utility model.

Claims (10)

1. a system that handles coal directly-liquefied residue is characterized in that, comprising:
(A) mixing tank has extraction solvent inlet, coal directly-liquefied residue inlet and coal liquefaction residue extraction mixture outlet at least;
(B) little omitted has at least
Coal liquefaction residue extraction mixture inlet, wherein, said coal liquefaction residue extraction mixture outlet is connected to coal liquefaction residue extraction mixture inlet,
Concentrate the outlet of coal liquefaction residue underflow, and
The outlet of clear liquor phase mixture;
(C) strainer has at least
Concentrate the import of coal liquefaction residue underflow, be connected to said concentrated coal liquefaction residue underflow outlet,
Filtrate outlet; And
(D) accurate filter has at least
Clear liquor phase mixture inlet is connected to said clear liquor phase mixture outlet,
The outlet of secondary filter clear filtrate, and
Outlet is mutually held back in secondary filter.
2. system according to claim 1, wherein, the filtrate outlet of said strainer and/or said secondary filter are held back to export mutually and are connected to said mixing tank.
3. system according to claim 1 further comprises: storage tank, the filtrate outlet of said strainer and/or said secondary filter are held back the said storage tank of outlet process mutually and are connected to said mixing tank.
4. according to each described system of claim 1 to 3; Wherein, Said little omitted comprises one or more little cyclone separators, and each little cyclone separator all has little cyclone separator inlet, little eddy flow concentrates underflow outlet and the outlet of clear liquor phase mixture.
5. according to each described system of claim 1 to 3, wherein, said little omitted is multistage little omitted.
6. system according to claim 5,
Wherein, the little cyclone separator inlet of the first step is as said coal liquefaction residue extraction mixture inlet; The little eddy flow of the first step concentrates the underflow outlet as said concentrated coal liquefaction residue underflow outlet;
Wherein, the outlet of the clear liquor phase mixture of the little cyclone separator of last step is as the clear liquor phase mixture outlet of said little omitted;
Wherein, the outlet of the underflow of little cyclone separator is connected to said mixing tank more than the second stage;
Wherein, the outlet of the clear liquor phase mixture of other each the little cyclone separator except that the little cyclone separator of last step is connected to the little cyclone separator inlet of next stage.
7. system according to claim 6, wherein, said little omitted is the little omitted of two-stage.
8. system according to claim 1, wherein, the concentrated coal liquefaction residue underflow outlet of said little omitted is connected to the concentrated coal liquefaction residue underflow import of said strainer via helix transporting device.
9. system according to claim 1, wherein, said coal liquefaction residue extraction mixture outlet is positioned at the bottom of said mixing tank, and is connected to the top of said mixing tank.
10. system according to claim 3, wherein, said storage tank is connected to said mixing tank via transh pump.
CN2011203713568U 2011-09-30 2011-09-30 System for treating coal direct liquefied residue Expired - Lifetime CN202246572U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399564A (en) * 2011-09-30 2012-04-04 神华集团有限责任公司 System and method for treating coal direct liquefaction residue
CN102730857A (en) * 2012-07-12 2012-10-17 华东理工大学 Method and device for closed separation of washing wastewater of reaction product and surplus heat utilization in isobutene preparation by dehydrogenation of isobutane
CN104004536A (en) * 2013-02-22 2014-08-27 神华集团有限责任公司 Mesophase pitch and preparation method thereof
CN106675626A (en) * 2017-01-18 2017-05-17 中石化炼化工程(集团)股份有限公司 Solid-liquid separation device for oil slurry and solid-liquid separation system for oil slurry

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399564A (en) * 2011-09-30 2012-04-04 神华集团有限责任公司 System and method for treating coal direct liquefaction residue
CN102399564B (en) * 2011-09-30 2014-05-21 神华集团有限责任公司 System and method for treating coal direct liquefaction residue
CN102730857A (en) * 2012-07-12 2012-10-17 华东理工大学 Method and device for closed separation of washing wastewater of reaction product and surplus heat utilization in isobutene preparation by dehydrogenation of isobutane
CN102730857B (en) * 2012-07-12 2014-07-30 华东理工大学 Method and device for closed separation of washing wastewater of reaction product and surplus heat utilization in isobutene preparation by dehydrogenation of isobutane
CN104004536A (en) * 2013-02-22 2014-08-27 神华集团有限责任公司 Mesophase pitch and preparation method thereof
CN104004536B (en) * 2013-02-22 2017-01-11 神华集团有限责任公司 Mesophase pitch and preparation method thereof
CN106675626A (en) * 2017-01-18 2017-05-17 中石化炼化工程(集团)股份有限公司 Solid-liquid separation device for oil slurry and solid-liquid separation system for oil slurry

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