The retracting device and recovery method of solvent in coal directly-liquefied residue extraction heavy phase
Technical field
The present invention relates to the recycling field of coal directly-liquefied residue, in particular to a kind of coal directly-liquefied residue extraction
Take the retracting device and recovery method of solvent in heavy phase.
Background technology
Direct coal liquefaction technology is in high temperature, high pressure, faces nitrogen atmosphere, and the coal in finite concentration coal is pyrolyzed, heat
Solution fragment carries out hydrogenation and further decomposition in the presence of catalyst, changes into the new of clean fuel liquid or industrial chemicals
Clean coal technology, is one of important directions of coal high-efficiency clean utilization technology.Invented in 1913 from German Bergius
Coal is hydrogenated with energy conversion solution oil product method under high temperature, high pressure, by the research and development in a century, DCL/Direct coal liquefaction skill
Art has been mature on the whole.Shenhua Erdos DCL/Direct coal liquefaction megaton demonstration project, drives successfully first from December, 2012
Since, Shenhua Group is in DCL/Direct coal liquefaction equipment technology, direct coal liquefaction process technology, DCL/Direct coal liquefaction catalyst technology, coal
Direct liquefaction sewage disposal technology, direct coal liquefaction technology engineering, direct coal liquefaction technology personnel training aspect all obtain huge
Quantum jump, current megaton demonstration project has been enter into the commercial operation stage.
Current all of direct coal liquefaction process, the conversion ratio of coal is impossible to reach 100%.Coal is being converted into liquid
While product, can also by-product account for the liquefied residue of feed coal 30%, they are mainly a kind of high-carbon, ash high, high-sulfur, high heating value
Material, be mainly made up of minerals in coal, catalyst, unconverted coal, asphaltene and heavy coal liquids.Wherein heavy coal liquids
25~30% or so are accounted for, the content of bitumen accounts for the 20~25% of level of residue, with not turning that solid form is present
Change coal, ash content and catalyst and account for 50% or so.No matter which kind of direct liquefaction technique is used, can all carry heavy in liquefied residue secretly
Liquefaction oil and bitumen.The separation of coal directly-liquefied residue directly affects the integrality and liquid of direct liquefaction technique with utilizing
This is melted into, is the key technical problem that coal high-efficiency direct liquefaction technique must be solved.
Chinese patent《The system and method for processing coal directly-liquefied residue》(CN102399564A), disclose a kind of to warp
The coal directly-liquefied residue crossed after extraction takes out method coupling and intensifying treatment coal directly-liquefied residue using mini-hydrocyclone separation device and solvent
Method and system, the concentration coal liquefaction residue that the method mini-hydrocyclone separation is obtained by the way of filter press press filtration, reclaim it is stagnant
The extractant stayed in concentration coal liquefaction residue, efficiency is low, and solvent recovery effect is poor.Chinese patent《One kind treatment coal is straight
The system for connecing liquefied residue》(CN202246573U), using the liquefaction oil of specific fraction section as extractant, to DCL/Direct coal liquefaction
Residue is extracted, and using cyclone separator and filter coupling technique, realizes consolidating for liquefied residue extract and extract remainder
Liquid separate, eddy flow residue concentrate resulting in the method, using it is hot pressurization coarse filtration after, then row blowback is carried out to filter cake
Dried process mode reclaims extractant, in view of insufficient to filtration cakes torrefaction, solvent recovering rate is low, and high concentration material is using filtering
Mode recycling design, efficiency is low.
As can be seen here, the extraction heavy phase that existing coal directly-liquefied residue is formed after solvent extraction, wherein the extraction for carrying
Taking solvent cannot effectively be reclaimed.Based on this, it is necessary to provide solvent in a kind of coal directly-liquefied residue extraction heavy phase
Retracting device.
The content of the invention
Retracting device it is a primary object of the present invention to provide solvent in a kind of coal directly-liquefied residue extraction heavy phase, with
Solve the problems, such as that the rate of recovery in the prior art for solvent in coal directly-liquefied residue extraction heavy phase is relatively low.
To achieve these goals, according to an aspect of the invention, there is provided a kind of coal directly-liquefied residue extraction weight
The retracting device of solvent in phase, it includes:Extraction heavy phase dilution unit, is provided with extraction heavy phase and enters in extraction heavy phase dilution unit
Mouth, extractant import and dilution material outlet;Solvent recovery unit, solvent recovery unit is used to carry out the solvent in dilution material
Vacuum spraying air lift is separated, and dilution material import and the outlet of gas phase material, dilution material import and dilution are provided with solvent recovery unit
Material outlet;And gas-liquid separation unit, gas phase material import, the import of gas phase material and gas phase material are provided with gas-liquid separation unit
Outlet.
Further, solvent recovery unit includes solvent recovery tower, sprayer is provided with solvent recovery tower, on sprayer
It is provided with dilution material import.
Further, gas distributor is additionally provided with solvent recovery tower, gas distributor is located at sprayer lower section, gas
Gas stripping gas import is provided with distributor.
Further, the bottom of towe end socket of solvent recovery tower is taper, and the outlet of solid phase material is provided with the cone angle of bottom of towe end socket.
Further, the cone angle ф of bottom of towe end socket is 30 °~120 °.
Further, rotary discharge valve is additionally provided with outside the bottom of towe of solvent recovery tower, rotary discharge valve and solid phase material go out
It is connected by discharge pipelines between mouthful.
Further, retracting device also includes preheater, and preheater is arranged between dilution material import and dilution material outlet
Pipeline on.
Further, gas-liquid separation unit includes:Condenser, is provided with the import of gas phase material on condenser and condensation material goes out
Mouthful;Knockout drum, be provided with knockout drum condensation material import, solvent outlet and separate gas outlet, condensation material outlet with
Condensation material inlet communication.
Further, gas-liquid separation unit also includes vavuum pump, and vavuum pump is arranged on the pipeline where separating gas outlet.
According to another aspect of the present invention, there is provided the recovery side of solvent in a kind of coal directly-liquefied residue extraction heavy phase
Method, it is comprised the following steps:Extraction heavy phase is diluted using extractant, obtains dilution material;Dilution material is carried out into vacuum
Spraying stripping process, obtains gas phase material and solid phase material;And gas phase material is carried out into gas-liquid separation, obtain separating gas and reclaim molten
Agent.
Further, in dilution material, extraction heavy phase accounts for the 40~75% of dilution material gross weight.
Further, 60 DEG C of viscosity of dilution material are less than 1000mpas.
Further, will dilution material carry out vacuum spraying stripping process the step of in, gas stripping gas using inert gas or
Organic fixed gas, it is preferred to use organic fixed gas.
Further, in the step of dilution material is carried out into vacuum spraying stripping process, the feeding temperature for diluting material is 100
~250 DEG C;The intake air temperature of gas stripping gas is 100~300 DEG C, and absolute pressure is less than 95KPa.
Further, the step of gas phase material being carried out into gas-liquid separation includes:Gas phase material is condensed, condensation material is obtained;
And
Condensation material is carried out into vacuum gas-liquid separation, obtains separating gas and recycling design.
Further, the temperature of condensation material is less than or equal to 54 DEG C.
In above-mentioned retracting device provided by the present invention, using extract heavy phase dilution unit can will extraction heavy phase carry out it is dilute
Release treatment, so as to get dilution material can realize solvent by way of vacuum spraying air lift in follow-up solvent recovery unit
Separation.Separated using the mode of the vacuum spraying air lift, can accumulate residue solid phase surface and minimize, balling-up is in Action of Gravity Field
Lower operation to solid phase material is exported.Then, after the gas phase material containing solvent composition being isolated to enters gas-liquid separation unit, energy
Reach solvent liquefaction therein and separate, reach and reclaim the purpose for extracting solvent in heavy phase, and separate gas stripping gas meeting
Exported from gas is separated.Different from other retracting devices, solvent recovery is carried out using the mode of vacuum spraying air lift in the present invention, its
Organic efficiency can be significantly improved.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing a further understanding of the present invention, of the invention to show
Meaning property and its illustrates, for explaining the present invention, not constitute inappropriate limitation of the present invention embodiment.In the accompanying drawings:
Fig. 1 shows the retracting device according to solvent in coal directly-liquefied residue extraction heavy phase in an embodiment of the present invention
Schematic diagram.
Wherein, above-mentioned accompanying drawing is marked including the following drawings:
10th, heavy phase dilution unit is extracted;20th, solvent recovery unit;21st, sprayer;22nd, gas distributor;23rd, rotary unloading
Material valve;30th, gas-liquid separation unit;31st, condenser;32nd, knockout drum;33rd, vavuum pump;40th, preheater.
Specific embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
As described by background technology, in the prior art for the recovery of solvent in coal directly-liquefied residue extraction heavy phase
Rate is relatively low.In order to solve this problem, the invention provides the recovery dress of solvent in a kind of coal directly-liquefied residue extraction heavy phase
Put, as shown in figure 1, it includes extraction heavy phase dilution unit 10, solvent recovery unit 20 and gas-liquid separation unit 30, extraction weight
The import of extraction heavy phase, extractant import and dilution material outlet are provided with phase dilution unit 10;Solvent recovery unit 20 is used to
Vacuum spraying air lift separation is carried out to the solvent in dilution material, dilution material import and gas phase material are provided with solvent recovery unit 20
Outlet, dilution material import and dilution material outlet;Be provided with gas phase material import in gas-liquid separation unit 30, the import of gas phase material and
Gas phase material outlet.
Term " coal directly-liquefied residue extraction heavy phase " herein refer to coal directly-liquefied residue after solvent extraction pass through from
The isolated heavy phase of mode such as heart separation, sedimentation separation.It is this area wherein for the solvent extraction of coal directly-liquefied residue
Well known to technical staff, will not be repeated here.
, can be diluted for extraction heavy phase using heavy phase dilution unit 10 is extracted by the above-mentioned retracting device that the present invention is provided
Treatment, so as to get dilution material can realize solvent by way of vacuum spraying air lift in follow-up solvent recovery unit 20
Separation.Residue solid phase surface product is minimized, and balling-up runs to the outlet of solid phase material under gravity.Then, it is isolated to
The gas phase material containing solvent composition enter gas-liquid separation unit 30 after, by solvent liquefaction therein and can separate, reach
To the purpose for reclaiming solvent in extraction heavy phase, and separate gas stripping gas can be exported from gas is separated.Different from other retracting devices,
Mode in the present invention using vacuum spraying air lift carries out solvent recovery, and its organic efficiency can be significantly improved.
In a kind of preferred embodiment, solvent recovery unit 20 includes solvent recovery tower, is provided with solvent recovery tower
Sprayer 21, is provided with dilution material import on sprayer 21.Dilution material can be converted into spray form using sprayer 21, by
The gas stripping of gas stripping gas under vacuum condition is crossed, solvent extraction in material can will be more effectively diluted out.Preferably, spray
The shower nozzle of device 21 includes but is not limited to pressure nozzle, rotating disk shower nozzle or double-current method shower nozzle.
Gas distributor 22, and gas distributor 22 are provided with a kind of preferred embodiment, in solvent recovery tower
In the lower section of sprayer 21, gas stripping gas import is provided with gas distributor 22.Can make gas stripping gas more using gas distributor 22
It is evenly distributed in tower, is more fully contacted with the dilution material of spray form, so as to further improves the rate of recovery of solvent.It is preferred that
Ground, gas distributor 22 including but not limited to the bottom of a pan disc type distributor, rung formula distributor or bubble cap distributor.
In a kind of preferred embodiment, the bottom of towe end socket of solvent recovery tower is taper, is set at the cone angle of bottom of towe end socket
There is solid phase material to export.Material is prevented from using taper low head to deposit, and be conducive to material collection.The cone angle of taper low head
ф is 30 °~120 °, preferably 30 °~90 °, further preferred 40 °~50 °.
In a kind of preferred embodiment, rotary discharge valve 23, rotary unloading are additionally provided with outside the bottom of towe of solvent recovery tower
It is connected by discharge pipelines between material valve 23 and the outlet of solid phase material.Rotary discharge valve 23 has the function of lock gas, using rotary unloading
Solid material inside material valve 23 and discharge pipelines and taper low head, is effectively formed gas sealing system, is the vacuum of dilution material
Air lift dries offer condition.Specifically, rotary discharge valve 23 also can be to lock the replacement such as gas blow-off valve, as long as it has lock airway dysfunction
.It is highly preferred that the length of discharge pipelines is 0.5~2.5m, diameter is not less than 50mm.
In actual mechanical process, the dilution material droplet containing solvent to be recycled through the dried powder material of vacuum air lift,
Under gravity, operation downwards, forms the material envelope of certain liquid level at taper low head and discharge pipelines.Simultaneously in rotation
In the presence of the lock gas of discharge valve 23, suitable vacuum condition is formed in solvent recovery tower, is conducive to the air lift of solvent to dry and separates,
More than the rotated discharge system of discharge valve 23 of the powder material of material position.
In a kind of preferred embodiment, retracting device also includes preheater 40, and preheater 40 is arranged on dilution material import
On the pipeline between dilution material outlet.Setting preheater 40 can make dilution material enter sprayer 21 at a higher temperature,
The high-temperature spray of formation can further improve the rate of recovery of solvent.
In a kind of preferred embodiment, gas-liquid separation unit 30 includes condenser 31 and knockout drum 32, condenser
The import of gas phase material and condensation material outlet are provided with 31;Condensation material import, solvent outlet are provided with knockout drum 32 and are divided
From gas outlet, condensation material import and condensation material outlet.The gas phase material that can be separated before using condenser 31 is condensed,
Solvent therein is condensed into liquid phase, realize being separated with gas stripping gas in knockout drum 32.It is highly preferred that gas-liquid separation list
Unit 30 also includes vavuum pump 33, and vavuum pump 33 is arranged on the pipeline where separating gas outlet.Gas-liquid can be made under vavuum pump 33
Separate more thorough.
In actual mechanical process, vavuum pump 33 is can to provide mechanical, injecting type of the pressure (absolute pressure) less than 95KPa
Or water-ring vacuum pump.Through the gas of the discharge system of vavuum pump 33, directly outer can arrange, can also be utilized in the system interior circulation, it is excellent
Anthology system interior circulation is utilized.
In addition, present invention also offers the recovery method of solvent in a kind of coal directly-liquefied residue extraction heavy phase, it includes
Following steps:Extraction heavy phase is diluted using extractant, obtains dilution material;Dilution material is carried out at vacuum spraying air lift
Reason, obtains gas phase material and solid phase material;And gas phase material is carried out into gas-liquid separation, obtain separating gas and recycling design.
The above-mentioned recovery method that the present invention is provided, place can be diluted using heavy phase dilution unit is extracted by extraction heavy phase
Reason, so as to get dilution material can be realized by way of vacuum spraying air lift in follow-up solvent recovery unit solvent point
From.Residue solid phase surface product is minimized, and balling-up runs to the outlet of solid phase material under gravity.Then, what is be isolated to contains
After the gas phase material for having solvent composition enters gas-liquid separation unit, by solvent liquefaction therein and can separate, reach recovery
The purpose of solvent in extraction heavy phase, and separate gas stripping gas can be exported from gas is separated.Different from other recovery methods, the present invention
The middle mode using vacuum spraying air lift carries out solvent recovery, and its organic efficiency can be significantly improved.
According to the above-mentioned teaching of the present invention, those skilled in the art can select specific operating procedure.A kind of preferred
Implementation method in, in above-mentioned dilution material, extraction heavy phase account for dilution material gross weight 40~75%, preferably account for 50%~65%.
Under the conditions of the ratio, dilution material has defeated good pipe, pumping, pulverability.It is highly preferred that 60 DEG C of viscosity of dilution material are less than
1000mpa·s.Specifically, extraction heavy phase can be using stirring, external pump size circulations also with effective homogeneous mixture of extractant
Or both are simultaneous the diversified forms such as to set, extraction heavy phase and the effective homogeneous mixture of extractant are realized.
In a preferred embodiment, in the step of dilution material is carried out into vacuum spraying stripping process, gas stripping gas
Using inert gas or organic fixed gas, it is preferred to use organic fixed gas.According to similar compatibility principle, organic fixed gas is in air lift
There is the rate of recovery higher during extractant.Specifically, inert gas can be nitrogen, argon gas etc., and organic fixed gas can
Think hydrogen, methane, ethane, propane or 2 kinds of above-mentioned substance or mixture of more than two kinds.
In a preferred embodiment, in the step of dilution material is carried out into vacuum spraying stripping process, dilution material
Feeding temperature be 100~250 DEG C;The intake air temperature of gas stripping gas is 100~300 DEG C, and absolute pressure is less than 95KPa.
In a preferred embodiment, the step of gas phase material being carried out into gas-liquid separation includes:Gas phase material is carried out cold
It is solidifying, obtain condensation material;And condensation material is carried out into vacuum gas-liquid separation, obtain separating gas and recycling design.
In a preferred embodiment, the temperature of condensation material is less than or equal to 54 DEG C.
The feeding temperature of above-mentioned dilution material, the temperature of gas stripping gas and vacuum can match regulation and control, can be in optimum condition
Lower completion extractant recovery operation.
Beneficial effects of the present invention are further illustrated with embodiment below:
Embodiment 1
Horizontal spiral separating and extracting heavy phase is entered into residue extraction heavy phase dilution unit, by extraction heavy phase:Extractant=
2:1 ratio adds extractant, carries out mixing and homogenizes, and obtains dilution material.The preheated device of dilution material is heated to 250 DEG C of entrance
Extractant recovery unit, under conditions of pressure (absolute pressure) is less than 95KPa hot nitrogen air lifts, carries out atomization drying, in gas-liquid
Separate vacuum tank collects extractant, and liquefied residue is discharged through the rotated discharge valve of powder material of dry solidification.Method extraction is molten
The rate of recovery of agent is more than 95%.
Comparative example 1
Horizontal spiral separating and extracting heavy phase is entered into blade dryer, blade drying is by 250 DEG C of conduction oil maintenance, in pressure
(absolute pressure) is dried less than under the conditions of 95KPa, and extractant is collected in extractant collecting tank, and liquefied residue is solid through drying
After change, discharge blade dryer extraction.The method recovery rate of extraction solvent is about 85%.
Comparative example 2
Horizontal spiral separating and extracting heavy phase is entered into thermal air pressure filtration filter, cleaner liquid (extractant) and filter residue was obtained
(residue solid slag charge), the method recovery rate of extraction solvent about 80% or so.
From data above, solvent recovery is carried out using retracting device of the invention, its solvent recovering rate is relatively remote high
In the rate of recovery of other retracting devices.It can thus be seen that above-mentioned retracting device provided by the present invention, using vacuum spraying gas
Carry and the solvent in coal directly-liquefied residue extraction heavy phase is reclaimed, it has the rate of recovery higher.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All any modifications within of the invention and principle, made,
Equivalent, improvement etc., should be included within the scope of the present invention.