CN107158744B - Extraction tower, extraction and separation system and coal tar extraction process - Google Patents

Extraction tower, extraction and separation system and coal tar extraction process Download PDF

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Publication number
CN107158744B
CN107158744B CN201610130000.2A CN201610130000A CN107158744B CN 107158744 B CN107158744 B CN 107158744B CN 201610130000 A CN201610130000 A CN 201610130000A CN 107158744 B CN107158744 B CN 107158744B
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extraction
solvent
inner cylinder
coal tar
sieve plate
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CN107158744A (en
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芦海云
陈爱国
孙任晖
赵帅
高鹏
刘爱国
郭屹
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China Energy Investment Corp Ltd
National Institute of Clean and Low Carbon Energy
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Shenhua Group Corp Ltd
National Institute of Clean and Low Carbon Energy
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0446Juxtaposition of mixers-settlers
    • B01D11/0457Juxtaposition of mixers-settlers comprising rotating mechanisms, e.g. mixers, mixing pumps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0426Counter-current multistage extraction towers in a vertical or sloping position
    • B01D11/0434Counter-current multistage extraction towers in a vertical or sloping position comprising rotating mechanisms, e.g. mixers, rotational oscillating motion, mixing pumps
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C1/00Working-up tar
    • C10C1/18Working-up tar by extraction with selective solvents

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Working-Up Tar And Pitch (AREA)

Abstract

The invention discloses a kind of extraction tower, extraction and separation system and coal tar extraction process, extraction tower includes the outer cylinder (5) and inner cylinder (4) of agitating device, filtering sieve plate (8) and nesting, and filtering sieve plate is removably mounted on inner cylinder bottom end.Extraction and separation system includes extraction tower and separative unit, separative unit includes extraction phase storage tank, separator, solvent tank and extract storage tank, the outer comb (11) of extraction phase, extraction phase storage tank and separator are sequentially connected, extraction phase is separated into extract and solvent by separator, and the solvent after separation is stored in solvent tank and can enter pipe (2) by solvent and backflows to inner cylinder.Extraction tower of the invention can be avoided blocking, convenient for safeguarding, can effectively slow down the air-teturning mixed phenomenon in extraction separation process.Extraction and separation system and technique can realize under temperate condition to lightweight in coal tar, heavy component and impurity it is quick, efficiently separate, reduce coke powder, coal dust and the inorganic mineral ingredient being rich in residual bitumen.

Description

Extraction tower, extraction and separation system and coal tar extraction process
Technical field
The invention belongs to extraction equipment and technology fields, particularly, are related to a kind of extraction tower apparatus and apply the extraction tower Extraction and separation technology for coal tar.
Background technique
Coal tar is the product liquid of coal brown obtained in heated destructive distillation or gasification or dark thick, simultaneously With penetrating odor.Coal tar nature is unstable, and comparison of ingredients is complicated, mainly by water, alkane, aromatic hydrocarbons and some contains Hetero atom (sulphur, nitrogen and oxygen) compound composition, and ingredient and content are with working condition (temperature, pressure, residence time, heating Rate, whether there is or not catalyst) variation it is very big.Coal tar mainly has 3 kinds of Land use systems at present: first is that directly burning or by adding hydrogen Handle the ready-mixed oil as petrol and diesel oil;Second is that retrofit becomes the intermediate products of all kinds of chemicals or dyestuff and medicine;Three It is to obtain asphaltic products and spin-off.
Above-mentioned coal tar utilization mostly establish formerly with distillation technique (including air-distillation and vacuum distillation two kinds of sides Formula) to coal tar carry out different fractions cutting, successively obtain light oil distillate (170 DEG C of <), carbolic oil fraction (170~230 DEG C), Wash oil fraction (230~300 DEG C), carbolineum fraction (270~360 DEG C) and pitch, different oil product fraction sections are respectively by adding hydrogen smart It makes, be hydrocracked the ready-mixed oil for obtaining fuel oil either petrol and diesel oil, and asphalt component can also lead in addition to building for reason Cross pitch coke modified or using delayed coking industrial production low-sulfur.But maximum temperature required for distillation technique reaches 450 DEG C or more, sometimes it is also contemplated that vacuum distillation, therefore, distillation technique the high requirements on the equipment, investment amount is big, Er Qieneng Consumption is also very big, in addition, coal tar also has the characteristics that high ash content, high viscosity, high-moisture simultaneously, has to pass through before distillation Certain processing makes solid content reduction meet distillation technique requirement, reduces load and subsequent handling that viscosity mitigates pump With reduction water content reduces the energy consumption of distillation.
Therefore, the thick object such as tar is carried out classification separation by a kind of method for needing to develop non-distillation, is reached in removing tar Solid waste, purpose that tar is separated.In known isolation technics, extraction and separation mode has been widely used in existing work During industry, but during the separation of the actual extraction of coal tar, sticky asphalitine and granular size unevenness in tar The presence of lime-ash often causes the blockage problem of equipment, extraction process is caused to be unable to operate stably, thus the structure of extraction equipment Selection with extractant is to realize the key point of extraction process reliability service.
Summary of the invention
It is in view of the above-mentioned drawbacks in the prior art or insufficient, the present invention provides a kind of extraction tower, extraction and separation system and Coal tar extraction process, the extraction tower can be avoided blocking, convenient for safeguarding, be conducive to the Rapid Extraction of each ingredient in coal tar, Separation, and extraction process is efficient, energy consumption is low.
To achieve the above object, according to an aspect of the invention, there is provided a kind of extraction tower, including agitating device, mistake Screen plate and the outer cylinder and inner cylinder of nested setting, are connected with that extract liquor enters pipe and solvent enters pipe on the top cover of extraction tower, The bottom of extraction tower is connected with the outer comb of extraction phase, and agitating device is protruded into inner cylinder and is stirred, and filtering sieve plate is removably pacified Mounted in the bottom end of inner cylinder using the bottom cover as the inner cylinder, so that the liquid in inner cylinder is outer via entering after the filtering of filtering sieve plate In cylinder.
Preferably, filtering sieve plate includes stacking and spaced multilayer mesh screen, and the screen-aperture of the multilayer mesh screen is from upper It is sequentially reduced under.
Preferably, filtering sieve plate further includes the filter membrane as interlayer, which is fixed at adjacent two layers of mesh Between sieve.
Preferably, which further includes the motor-driven mechanism being arranged in above top cover, which passes through Elevating lever is connected with filtering sieve plate, and under the lifting driving of motor-driven mechanism, filtering sieve plate can be upwardly against inner cylinder Bottom end, or move down to be disconnected with inner cylinder.
Preferably, agitating device includes blade and rotating bar, and blade is mounted on the bottom end of rotating bar and protrudes into inner cylinder, is turned The top of lever is connected can be driven to rotate with motor-driven mechanism.
Preferably, rotating bar is hollow stem, and elevating lever is co-axially located in rotating bar.
Preferably, inner cylinder integrally protrudes into outer cylinder, and top cover covers the top of inner barrel and outer barrel simultaneously.
Preferably, at least part of inner cylinder stretches out in outer cylinder upwards, and the top of the outer cylinder is circumferentially connected to the outer of inner cylinder Barrel, top cover are sealed on the top of inner cylinder.
According to another aspect of the present invention, a kind of extraction and separation system is provided, including separative unit and above-mentioned extraction Tower, separative unit include extraction phase storage tank, separator, solvent tank and extract storage tank, extraction phase outer comb, extraction phase storage tank It is sequentially connected with separator, the extraction phase of extraction tower discharge is separated into extract and solvent by separator, the extraction after separation Object is stored in extract storage tank, and the solvent after separation is stored in solvent tank and can enter pipe by solvent and backflows to interior In cylinder.
Preferably, which includes multiple separative units, and the outer comb of extraction phase is equipped with multiple-way valve, to pass through Multiple-way valve is separately connected multiple separative units.
The present invention further correspondingly provides a kind of coal tar extraction process, using above-mentioned extraction and separation system, coal tar extraction Taking technique includes extraction step: the coal tar after preheating and stirring being passed through extraction tower, and is passed through predetermined quality ratio Solvent is stirred extraction, obtains extract and recycling design by separative unit after extraction tower extraction.
Preferably, in extraction step, the solvent for being passed through extraction tower is preheated, and be passed through extraction tower coal tar it is pre- Heating temperature is not more than 120 DEG C.
Preferably, extraction step includes the multitple extraction to coal tar, is passed through in every grade of extraction into extraction tower different Solvent, and by extract corresponding with the connected different separative unit acquisitions of extraction tower and recycle corresponding solvent.
Preferably, in multitple extraction, the dissolubility for the solvent that rear class extraction uses is higher than prime and extracts the solvent used Dissolubility.
It is highly preferred that extraction step includes level-one extraction and second level extraction, in level-one extraction the solvent that uses for petroleum ether, Light oil or washing oil, the solvent that uses is arene compounds, acetone or tetrahydrofuran in second level extraction.
Preferably, extraction step includes that recovered solvent is flowed back into extraction tower by separative unit.
Particularly, coal tar extraction process further include filtering extraction step: filtering sieve plate blocking when, decline filtering sieve plate with It is separated with inner cylinder, stop being passed through coal tar and increases the intake of solvent, under the stirring action of agitating device, by the miscellaneous of blocking Matter flows into outer cylinder with solvent.
Particularly, coal tar extraction process further includes filtering sieve plate cleaning: by the emptying rate of liquid in extraction tower, incited somebody to action Screen plate is separated with inner cylinder, inner cylinder is separated with outer cylinder, is taken out filtering sieve plate and is cleaned.
According to the above technical scheme, it is used in extraction tower of the invention and opens the double-barrel structure unloaded and filtering sieve plate, because And in extraction process, filtering the impurity blocked in sieve plate can be also dismountable when needed by solvent washing, to avoid blocking Inner/outer tube and filtering sieve plate to achieve the purpose that exterior clean, get rid of in extraction process due to bitumen content is excessively high and with it is miscellaneous The phenomenon that matter forms thick object and filter screen is caused to block slows down the period that blocking occurs, alleviates the blocking bring repair time. Double-barrel structure design can effectively slow down the air-teturning mixed phenomenon in extraction separation process.In extraction and separation system and technique, it can be achieved that Under temperate condition to light components in coal tar, heavy component and impurity it is quick, efficiently separate, reduce rich in remaining pitch Containing coke powder, coal dust and the inorganic mineral ingredient in original coal tar, the pitch of acquisition is by easy method processing as weight The carbon material raw material wanted come using.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is a kind of structural schematic diagram of the extraction tower of preferred embodiment according to the present invention;
Fig. 2 is the structural schematic diagram of the extraction tower of another preferred embodiment according to the present invention;
Schematic diagram when Fig. 3 is the filtering sieve plate decentralization deslagging in extraction tower shown in FIG. 1;
Process schematic when Fig. 4 a~Fig. 4 e is the filtering sieve plate replacement in extraction tower shown in FIG. 1;
Fig. 5 is the schematic diagram according to the extraction and separation system of the preferred embodiment of the present invention.
Description of symbols
1 motor-driven mechanism, 2 solvent enters pipe
3 extract liquors enter 4 inner cylinder of pipe
5 outer cylinder, 6 top cover
7 elevating levers 8 filter sieve plate
9 rotating bar, 10 blade
11 extraction phases, 41 outer tube wall of outer comb
21 first extraction phase storage tank, 22 second extraction phase storage tank
31 first separator, 32 second separator
41 first solvent tank, 42 second solvent tank
51 first extract storage tank, 52 second extract storage tank
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
In the present invention, in the absence of explanation to the contrary, the noun of locality used such as " upper and lower, top, bottom " is usually needle For direction shown in the drawings either for it is vertical, on vertical or gravity direction for each component mutual alignment relation Word is described;" vertical direction " refers to the paper up and down direction of diagram;" inside and outside " is commonly referred to as chamber Inside and outside chamber.
As depicted in figs. 1 and 2, the present invention provides a kind of extraction tower, which includes agitating device, filtering sieve plate 8 And nested outer cylinder 5 and inner cylinder 4, it is connected with that extract liquor enters pipe 3 and solvent enters pipe 2, extraction tower on the top cover 6 of extraction tower Bottom be connected with the outer comb 11 of extraction phase, agitating device is protruded into inner cylinder 4 and is stirred, and filtering sieve plate 8 is removably installed In the bottom end of inner cylinder 4 using the bottom end opening of the bottom cover covering inner cylinder 4 as the inner cylinder 4, so that the liquid in inner cylinder 4 is via filtering Enter in outer cylinder 5 after the filtering of sieve plate 8.The filtering sieve plate 8 of liftable dismounting is additionally arranged in extraction equipment of the invention, with needle To the ingredient properties of coal tar, the lime-ash etc. of asphalitine therein Yu granular size unevenness is effectively filtered out, various impurity is avoided to produce Raw blocking.It is designed in addition, using double-barrel structure in extraction equipment of the invention, can effectively slow down returning in extraction separation process Mixed phenomenon.Therefore, extraction tower of the invention is particularly suitable for the high extraction solution of the impurity contents such as coal tar, gets rid of and is extracting It is convenient for safeguarding in the process since bitumen content is excessively high and the phenomenon that forming thick object with impurity and filter screen is caused to block, and equipment Low cost, less investment, payoff period are short, remarkable benefit.
Filtering sieve plate 8 to screen-aperture can be determined according to the particle size of the impurity component of extraction liquids.Filter screen Plate 8 can be single layer structure, but in the present embodiment, preferably use multilayered structure, i.e., filtering sieve plate 8 include stacking and Every the multilayer mesh screen (as shown in fig 4e) of setting, the screen-aperture of the multilayer mesh screen is sequentially reduced from top to bottom, successively to filter Different size of impurity.Further, filtering sieve plate 8 may also include the filter membrane (not shown) as interlayer, the filtering Film is fixed between two layers adjacent of mesh screen.By the way that filter membrane is arranged, more small impurity can be removed.
In the present embodiment, to be controlled convenient for the operation to filtering sieve plate 8, by filtering sieve plate 8 and agitating device one Installation.Referring to Fig. 1 or Fig. 2, extraction tower includes the motor-driven mechanism 1 that 6 top of top cover is arranged in, and motor-driven mechanism 1 passes through Elevating lever 7 is connected with filtering sieve plate 8.Therefore, under the lifting driving of motor-driven mechanism 1, filtering sieve plate 8 can such as Fig. 1 and It is upwardly against the bottom end of inner cylinder 4 as shown in Figure 2, can also move down as illustrated in fig. 3 to be disconnected with inner cylinder 4.
Except motor-driven mechanism 1, agitating device further includes blade 10 and rotating bar 9, and blade 10 is mounted on the bottom of rotating bar 9 It holds and protrudes into inner cylinder 4, the top of rotating bar 9 is connected can be driven to rotate with motor-driven mechanism 1.Preferably, it rotates Bar 9 is hollow stem, and elevating lever 7 is co-axially located in rotating bar 9.Therefore, motor-driven mechanism 1 can drive elevating lever 7 simultaneously Filtering sieve plate 8 and 9 elevating movement of rotating bar are driven, rotating bar 9 can also be independently with 10 rotary motion of movable vane piece to be stirred Operation avoids generating any mechanical interference between two bars.Wherein, this motor driven machine for having rotation driving and Linear Driving Structure 1 usually may include motor, reduction gearbox, gear-box etc. in composition, and gear-box may include rotary drive gear, feed screw nut's biography Motivation structure etc..The top of rotating bar 9 can be fixedly installed with the circumferential gear with rotary drive gear cooperation, along rotating bar 9 The circumferential intermeshing of cross section, so that rotating bar 9 be driven to rotate.The rotation of motor driven screw rod, the fixed peace in the top of elevating lever 7 Loaded on feed screw nut, to constitute screw nut driving mechanism, 7 lifting moving of elevating lever is driven.This motor driven machine The rotation driving of structure 1 and the structure composition of Linear Driving are well known to those skilled in the art, and the structure emphasis of non-present invention, Thus it is not described further in detail.
In addition, being sufficiently stirred in inner cylinder 4 in the double-barrel structure of extraction tower, the liquid of the heavier mass after stirring Body is sunk down into the inner cavity of outer cylinder 5, since barrel dliameter is different and the presence of spaced walls, can effectively be slowed down in extraction separation process Air-teturning mixed phenomenon improves extraction efficiency.Wherein, as a kind of preferred constructive form, in extraction tower shown in Fig. 2, inner cylinder 4 is whole to be stretched Enter in outer cylinder 5, and top cover 6 covers the top of inner cylinder 4 and outer cylinder 5 simultaneously.And in extraction tower shown in Fig. 1, one of inner cylinder 4 Divide and stretch out in outside outer cylinder 5 upwards, the top of the outer cylinder 5 is circumferentially connected to the outer tube wall 41 of inner cylinder 4, and top cover 6 is sealed on inner cylinder 4 Top.It can be connected by modes such as bolt, screw or Tenons between inner cylinder 4 and outer cylinder 5 or bearing seat type is engaged by clamping, realized removable Formula installation is unloaded, also settable sealing ring is when necessary to carry out circumferential sealing in junction.
As shown in figure 3, when being extracted using extraction tower shown in FIG. 1 to coal tar, if solid particle or tar When sieve plate 8 is filtered in asphalitine blocking in component, rotating bar 9 can be controlled by motor-driven mechanism 1 and declined, make to filter sieve plate 8 It is separated with inner cylinder 4, is then shut off extract liquor and enters the stopping of pipe 3 and be passed through coal tar, and further increase solvent flux.Meanwhile then Rotated by 1 driving blade 10 of motor-driven mechanism, thus under the action of rotating fluid, make to block the impurity of screen plate 8 with Solvent flows out to outer cylinder 5 from the circumferential gap between filtering sieve plate 8 and inner cylinder 4, and then is discharged through comb 11 outside extraction phase.
As shown in Fig. 4 a~4e, when blocking is serious, needs that filtering sieve plate 8 is safeguarded, replaced, it can pass sequentially through and tear open Except fasteners such as bolts, so that outer cylinder 5 is separated with inner cylinder 4;Then elevating lever 7 is set to drive filter screen by motor-driven mechanism 1 Plate 8, rotating bar 9, blade 10 decline, and filtering sieve plate 8 is disconnected with inner cylinder 4;It again will filtering sieve plate 8 and rotating bar 9, elevating lever Filtering sieve plate 8 is removed in 7 separation;Finally by remove filtering sieve plate 8 different pore size multilayer mesh screen remove, using rinse or The mode that person burns removes the impurity being adhered on sieve.If there is filter membrane, need first to remove filter membrane, in order to avoid cause membrane body Damage.
On the basis of above-mentioned extraction tower, the present invention also provides a kind of extraction and separation system, which may include and extracts The separative unit for taking tower to connect, separative unit includes extraction phase storage tank, separator, solvent tank and extract storage tank, extraction phase Outer comb 11, extraction phase storage tank and separator are sequentially connected, and the extraction phase of extraction tower discharge is separated into extract by separator And solvent, the extract after separation are stored in extract storage tank, the solvent after separation is stored in solvent tank and can lead to It crosses solvent and enters pipe 2 and backflow into inner cylinder 4.
In the extraction and separation system, extraction tower bottom liquid extracted (i.e. extraction phase) passes through the outer comb 11 of extraction phase It is expelled to separative unit, extract and solvent further may separate out by separator, the extract after separation is extracted into extraction It takes in object storage tank, the solvent after separation can be entered pipe 2 by solvent and be backflowed into inner cylinder 4, recycling, participate in extracting repeatedly Journey.
Wherein, which may include multiple separative units, and the outer comb 11 of extraction phase is equipped with multiple-way valve, with logical It crosses multiple-way valve and is separately connected multiple separative units, to can realize that different solvents extract the series classification of extract liquor.Such as Fig. 5 Shown in include mutually independent two separative units, it can be achieved that two-stage extraction and separation in extraction and separation system.
Finally, the present invention also provides a kind of coal tar extraction process according to above-mentioned extraction tower and extraction and separation system, it should Technique includes at least extraction step: the coal tar after preheating and stirring entered into pipe 3 by extract liquor and is passed through extraction tower, and Enter pipe 2 by solvent and be passed through the solvent of predetermined quality ratio and be stirred extraction, is stirred repeatedly in extraction tower, stood After extraction, the extraction phase of bottom is separated by separative unit again, obtains extract and recycling design.Wherein, pass through separative unit Also recovered solvent can be entered pipe 2 by solvent from solvent tank and flow back into extraction tower, to improve the utilization rate of solvent.
It is important to note that the solvent for being passed through extraction tower is also preferably preheated in above-mentioned extraction step, The preheating temperature upper limit is the boiling point of the solvent.The pre-heating temperature for being passed through the coal tar of extraction tower can be not more than 120 DEG C, relative to It needs for the distillation extraction technique of higher pre-heating temperature (< 450 DEG C), it can be achieved that in a mild condition to light in coal tar Matter component, heavy component and impurity it is quick, efficiently separate, and then provide reliable original for the high value added utilization of coal tar Material.
When there are multiple independent separative units, above-mentioned extraction step may include the multitple extraction to coal tar, every grade Different solvents is passed through in extraction into extraction tower, and passes through extraction corresponding with the connected different separative unit acquisitions of extraction tower It takes object and recycles corresponding solvent.In multitple extraction, the dissolubility for the solvent that rear class extraction uses should be higher than that prime extraction makes The dissolubility of solvent is obtained more active principles with extraction and separation, and removes more impurity.
For coal tar, light components, heavy component and residue can be divided into, thus above-mentioned extraction step can be divided into one Grade extraction and second level extraction.Certainly, multitple extraction, isolated more components can also be carried out as needed.When progress Fig. 5 institute When the two-stage extraction shown, according to dissolubility power, the selection of solvent is generally with alkanes, aromatic hydrocarbons and dissolubility extremely strong third The sequence of ketone, tetrahydrofuran or pyridine carries out extraction.Therefore the solvent used in level-one extraction is preferably petroleum ether, light oil or washes Oil etc., the solvent that uses is selected as arene compounds, acetone or the tetrahydrofurans such as the stronger toluene of melting property etc. in second level extraction.
Require coal tar under the pretreatment condition for being sufficiently stirred and heating when level-one extracts, temperature is less than 120 DEG C, coal tar Oil is mixed with solvent 1 according to the mass ratio of 1:1~3, is extracted 10-30 minutes, obtains extraction phase, extraction via filtering sieve plate 8 It is mutually temporarily stored into the first extraction phase storage tank 21, extract remainder is tar light composition, and extraction phase is isolated by the first separator 31 Containing coke powder, coal dust, inorganic mineral tar heavy asphalt, be stored in the first extract storage tank 51, while to extraction phase First solvent can be recycled after being distilled, and recycle.
Require tar under the pretreatment condition for being sufficiently stirred, heating when second level extracts, temperature is less than 120 DEG C, to level-one Secondary solvent, extract remainder and secondary solvent are added in extract remainder after the completion of extraction to mix according to the mass ratio of 1:1~3, extraction It takes 10-30 minutes, is temporarily stored into the second extraction phase storage tank 22 via the extraction phase of sieve plate filtering 8, is divided by the second separator 32 From acquisition secondary solvent and second level extract;Extract herein is generally the purification ingredient in coal tar, is stored in the second extraction It takes in object storage tank 52;Extract remainder on sieve plate is almost impurity all in tar;Extract is distilled, to recycle second level molten Agent is recycled.
As it can be seen that the presence of the impurity component insoluble in solvent due to coal tar, above-mentioned coal tar extraction process further include Filter extraction step: when filter screen plate 8 generates blocking, for decline filtering sieve plate 8 to separate with inner cylinder 4, stopping is passed through coal tar And increase the intake of solvent, under the stirring action of agitating device, the impurity of blocking is flowed into outer cylinder 5 with solvent, such as Fig. 3 It is shown.In addition, it may further comprise filtering sieve plate cleaning as shown in Fig. 4 a~4e: by the emptying rate of liquid in extraction tower, incited somebody to action Screen plate 8 is separated with inner cylinder 4, inner cylinder 4 is separated with outer cylinder 5, is taken out filtering sieve plate 8 and is cleaned.It is walked by this filtering deslagging Rapid and filtering sieve plate cleaning, avoids the generation of clogging, facilitates going on smoothly for extraction process, facilitates device dimension Shield.
Therefore, after completing above-mentioned second level extraction, it can get extract remainder by extracting filtering sieve plate 8, i.e., own in tar The impurity such as coal dust, coke powder, inorganic mineral and a small amount of quinoline insolubles.Specifically, by opening filter screen plate 8, using a small amount of Light oil or carbolineum wash sieve plate, make crack place discharge of the impurity through sieve plate and extraction cylinder inner wall, in order to avoid blocking sieve plate Influence filter effect.
Extraction tower, extraction and separation system and technique through the invention, can (highest extraction temperature < in a mild condition 120 DEG C) and condition of normal pressure under complete extraction and separation to coal tar, reduce in remaining pitch rich in original coal tar The pitch of coke powder, coal coal and inorganic mineral ingredient, the hydrogenated available light oil of the extract of acquisition, acquisition passes through simplicity Method processing as important carbon material raw material come using.
Embodiment 1: entering the inner cylinder 4 that pipe 3 is delivered to extraction tower through extract liquor for 80 DEG C or so of coal tar, with equal flows Normal heptane be solvent, make the mass ratio 1:1 of the coal tar and solvent in the inner cylinder 4 of extraction tower, motor-driven mechanism 1 is with turn Lever 9 and blade 10 are constantly in whipping process, are opened the outlet valve of extraction tower being located in the outer comb 11 of extraction phase, are made to extract It takes and mutually enters in the first extraction phase storage tank 21, extraction phase is divided into normal heptane through the first separator 31 (such as distillation separator) and enters In first solvent tank 41, extract stores in the first extract storage tank 51, the normal heptane circulation in the first solvent tank 41 Into being extracted in extraction tower, after normal heptane is recycled 3 times, the normal heptane extract that is obtained in the first extract storage tank 51 Accounting for crude tar mass percent is 35.2;
Be toluene by solvent replacement, toluene enters the inner cylinder 4 that pipe 2 enters extraction tower through solvent, make tar in inner cylinder 4 and Solvent quality ratio 1:1, motor-driven mechanism 1 drive rotating bar 9 and blade 10 to be constantly in stirring, open the extraction of extraction tower The outlet valve in the outer comb 11 of phase is taken, enters extraction phase in the second extraction phase storage tank 22, extraction phase (is steamed through the second separator 22 Evaporate separator) it is divided into toluene into the second solvent tank 42, extract stores in the second extract storage tank 52, the second solvent Toluene in storage tank 42, which is recycled into extraction tower, to be extracted, and after toluene recycles 3 times, obtains first in the second extract storage tank 52 It is 57.1 that benzene extract, which accounts for crude tar mass percent,;
Opening motor-driven mechanism 1 separates filtering sieve plate 8 with the bottom end of inner cylinder 4, and light oil is added and carries out to filtering sieve plate 8 Cleaning, it is 7.7 that isolated toluene insoluble substance (predominantly asphalitine, cinder, minerals etc.), which accounts for crude tar mass percent,.
Embodiment 2: entering the inner cylinder 4 that pipe 3 is delivered to extraction tower through extract liquor for 50 DEG C or so of coal tar, with equal flows Normal heptane be solvent, make tar and solvent quality ratio 1:1 in inner cylinder 4, drive rotating bar 9 and blade 10 to locate always by motor In stirring, extraction tower outlet valve is opened, extraction phase enters in the first extraction phase storage tank 21, and extraction phase is through the first separator 31 It is divided into normal heptane to enter in the first solvent tank 41, extract stores in the first extract storage tank 51, the first solvent tank 41 In normal heptane be recycled into extraction tower and extracted, after normal heptane recycles 3 times, obtain positive heptan in the first extract storage tank 51 It is 84.2 that alkane extract, which accounts for crude tar mass percent,;
It is toluene by solvent replacement, toluene enters pipe 2 through solvent and enters inner cylinder 4, makes tar and solvent quality in inner cylinder 4 Than 1:1, motor drives rotating bar 9 and blade 10 to be constantly in whipping process, opens extraction tower outlet valve, and extraction phase enters the In two extraction phase storage tanks 22, extraction phase divides through the second separator 22 and enters in the second solvent tank 42 for toluene, and extract is the It is stored in two extract storage tanks 52, the toluene in the second solvent tank 42, which is recycled into extraction tower, to be extracted, toluene circulation 3 Obtaining toluene extract after secondary, in the second extract storage tank 52 and accounting for crude tar mass percent is 13.9;
Opening motor-driven mechanism 1 separates filtering sieve plate 8 with the bottom end of inner cylinder 4, and light oil is added and carries out to filtering sieve plate 8 Cleaning, it is 1.9 that isolated toluene insoluble substance (predominantly asphalitine, cinder, minerals etc.), which accounts for crude tar mass percent,.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited to above-mentioned realities The detail in mode is applied, within the scope of the technical concept of the present invention, various letters can be carried out to technical solution of the present invention Monotropic type, such as filtering sieve plate 8 is not limited to install together with agitating device and by same motor driven, filtering sieve plate 8 can also It is independently arranged, to realize convenient detachable installation;These simple variants are fallen within the protection scope of the present invention.
Each particular technique feature described in above-mentioned specific embodiment can pass through in the case of no contradiction Any suitable way is combined, and in order to avoid unnecessary repetition, the present invention is no longer another to various combinations of possible ways Row explanation.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (17)

1. a kind of extraction tower, outer cylinder (5) and inner cylinder (4) including agitating device, filtering sieve plate (8) and nested setting are described It is connected with that extract liquor enters pipe (3) and solvent enters pipe (2) on the top cover (6) of extraction tower, the bottom of the extraction tower is connected with The outer comb (11) of extraction phase, the agitating device are protruded into the inner cylinder (4) and are stirred, and the filtering sieve plate (8) is detachable Ground is mounted on the bottom end of the inner cylinder (4) using the bottom cover as the inner cylinder (4), so that the liquid in the inner cylinder (4) is via institute Enter in the outer cylinder (5) after stating the filtering of filtering sieve plate (8), wherein the extraction tower further includes being arranged in the top cover (6) The motor-driven mechanism (1) of top, the motor-driven mechanism (1) are connected by elevating lever (7) with the filtering sieve plate (8), Under the lifting driving of the motor-driven mechanism (1), filtering sieve plate (8) can be upwardly against the bottom of the inner cylinder (4) End, or move down to be disconnected with the inner cylinder (4).
2. extraction tower according to claim 1, wherein the filtering sieve plate (8) includes stacking and spaced multilayer The screen-aperture of mesh screen, mesh screen described in the multilayer is sequentially reduced from top to bottom.
3. extraction tower according to claim 2, wherein filtering sieve plate (8) further includes the filter membrane as interlayer, should Filter membrane is fixed between the mesh screen of adjacent two layers.
4. extraction tower according to claim 1, wherein the agitating device includes blade (10) and rotating bar (9), described Blade (10) is mounted on the bottom end of the rotating bar (9) and protrudes into the inner cylinder (4), the top of the rotating bar (9) and institute Motor-driven mechanism (1) is stated to be connected can be driven to rotate.
5. extraction tower according to claim 4, wherein the rotating bar (9) is hollow stem, and the elevating lever (7) is coaxial Setting is in the rotating bar (9).
6. extraction tower according to claim 1, wherein the inner cylinder (4) is integrally protruded into the outer cylinder (5), and described Top cover (6) covers the top of the inner cylinder (4) and outer cylinder (5) simultaneously.
7. extraction tower according to claim 1, wherein at least part of the inner cylinder (4) stretches out in described outer upwards Cylinder (5), the top of the outer cylinder (5) are circumferentially connected to the outer tube wall (41) of the inner cylinder (4), and the top cover (6) is sealed on described The top of inner cylinder (4).
8. a kind of extraction and separation system, including separative unit and according to claim 1~any one of 7 described in extraction tower, The separative unit includes extraction phase storage tank, separator, solvent tank and extract storage tank, the outer comb (11) of the extraction phase, The extraction phase storage tank and the separator are sequentially connected, and the extraction phase of the extraction tower discharge is separated by the separator Extract and solvent, the extract after separation are stored in the extract storage tank, and the solvent after separation is stored in It pipe (2) can be entered in the solvent tank and by the solvent backflows into the inner cylinder (4).
9. extraction and separation system according to claim 8, wherein the extraction and separation system includes that multiple separation are single Member, the outer comb (11) of the extraction phase is equipped with multiple-way valve, to be separately connected multiple separative units by the multiple-way valve.
10. a kind of coal tar extraction process, using extraction and separation system according to claim 8 or claim 9, the coal tar extraction Taking technique includes extraction step: the coal tar after preheating and stirring being passed through the extraction tower, and is passed through predetermined mass ratio The solvent of rate is stirred extraction, obtains extract and recycling design by the separative unit after extraction tower extraction.
11. coal tar extraction process according to claim 10, wherein in the extraction step, to being passed through the extraction The solvent of tower is preheated, and the pre-heating temperature for being passed through the coal tar of the extraction tower is not more than 120 DEG C.
12. coal tar extraction process according to claim 10, wherein the extraction step includes to the coal tar Multitple extraction, every grade extraction in different solvents, and the difference by being connected with the extraction tower are passed through into the extraction tower The separative unit obtain corresponding extract and recycle the corresponding solvent.
13. coal tar extraction process according to claim 12, wherein in multitple extraction, rear class extraction uses molten The dissolubility of agent is higher than the dissolubility for the solvent that prime extraction uses.
14. coal tar extraction process according to claim 13, wherein the extraction step includes level-one extraction and second level It extracts, the solvent used in the level-one extraction is petroleum ether, light oil or washing oil, and the solvent used in the second level extraction is virtue Hydrocarbon compound, acetone or tetrahydrofuran.
15. coal tar extraction process according to claim 10, wherein the extraction step includes single by the separation The solvent of recycling is flowed back into the extraction tower by member.
16. coal tar extraction process described in any one of 0~15 according to claim 1, wherein the coal tar extracts work Skill further includes filtering extraction step: when the filtering sieve plate (8) blocks, the decline filtering sieve plate (8) with the inner cylinder (4) Separation stops being passed through the coal tar and increasing the intake of the solvent to block up under the stirring action of the agitating device The impurity of plug flows into the outer cylinder (5) with the solvent.
17. coal tar extraction process described in any one of 0~15 according to claim 1, wherein the coal tar extracts work Skill further includes filtering sieve plate cleaning: by the emptying rate of liquid in the extraction tower, by the filtering sieve plate (8) and the inner cylinder (4) separation, the inner cylinder (4) are separated with outer cylinder (5), are taken out the filtering sieve plate (8) and are cleaned.
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CN107931101A (en) * 2017-11-17 2018-04-20 季梅 A kind of continuous travelling sieve material device
KR102428396B1 (en) * 2018-05-08 2022-08-02 오씨아이 주식회사 Method for treating high solid coal tar
CN109133004B (en) * 2018-09-25 2022-02-25 浙江工业职业技术学院 Hydrogen manufacturing equipment for hydrogen energy power automobile
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