CN108410491A - A kind of method and system preparing pitch using coal liquefaction residue - Google Patents
A kind of method and system preparing pitch using coal liquefaction residue Download PDFInfo
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- CN108410491A CN108410491A CN201810212523.0A CN201810212523A CN108410491A CN 108410491 A CN108410491 A CN 108410491A CN 201810212523 A CN201810212523 A CN 201810212523A CN 108410491 A CN108410491 A CN 108410491A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The present invention relates to a kind of method and systems preparing pitch using coal liquefaction residue.Including, hybrid extraction device, the first filter element, the second filter element, drying device and distilling apparatus, the hybrid extraction device is connected to first filter element, first filter element is connected to the drying device, first filter element is connected to second filter element, second filter element is connected to the distilling apparatus, wherein, first filter element includes at least the first filter device and the second filter device, and the second filter element includes at least third filter device and the 4th filter device.Pitch preparation system provided by the invention, includes two filter devices in two filter elements, and filter device alternately, realizes the continuous production of pitch.
Description
Technical field
The invention belongs to coal field of deep, and in particular to a kind of processing method of coal directly-liquefied residue, especially
Be related to a kind of coal directly-liquefied residue to after fully extracting be separated by solid-liquid separation so that obtain refined bitumen method and
System.
Background technology
China is rich in coal and poor in oil, and energy security situation is serious.DCL/Direct coal liquefaction be exactly at high temperature under high pressure, it is molten by means of hydrogen supply
Agent and catalyst make protium enter the molecular structure of coal and its derivative, to convert coal to liquid fuel or chemical industry
The advanced clean coal technology of raw material.Development of coal liquefaction technology is to alleviate China's oil shortage of resources, oil product supply and demand anxiety
One of important channel of situation, while being also to improve coal resources in China utilization rate, mitigate pollution that caused by coal burning, promote the energy, economy,
The important measures of harmonious development.
In DCL/Direct coal liquefaction production process, which kind of direct coal liquefaction process, the conversion ratio of coal is either used all can not
100% can be reached, finally always have a small amount of unconverted coal that liquefying plant need to be discharged, in addition the inorganic mineral carried secretly in coal and addition
The catalyst of coal slurry, they are mixed with solid forms and liquefaction oil.Various liquefaction process use different solid-liquids
Separation separation method separates they and liquefaction oil, and it is several to common are vacuum distillation, solvent extraction and filtering etc..Separate liquefaction
Solid matter after oil is known as coal directly-liquefied residue, referred to as coal liquefaction residue.
The property of coal liquefaction residue depends on type, liquefaction process condition and the solid-liquid separating method of liquefaction coal, it is one
The substance of the high charcoal of kind, high ash, high-sulfur, yield commonly reach 30% of feed coal or so.The appearance of coal liquefaction residue at room temperature
In solid asphalt shape, softening point is about 180 DEG C or so.Coal liquefaction residue includes heavy coal liquids, bitumen, unconverted coal
With additional catalyst, wherein heavy coal liquids and bitumen content account for about 50% of residue or so, unconverted coal and account for about
30% or so, ash content about 20% or so.Either from the whole economy of liquefaction, or from the angle of the utilization of resources and environmental protection
Degree sets out, and is required for being processed liquefied residue and trans-utilization, this is also that coal high-efficiency direct liquefaction technique is necessary
One of key technical problem of solution.Heavy coal liquids and bitumen in residue are readily dissolved in organic solvent, using having
The method of solvent extraction carries out sub-prime classified utilization to coal liquefaction residue, has important economic benefit and social benefit.
Solvent extraction is carried out to coal liquefaction residue, then carries out separation of solid and liquid and solvent recovery, there is following difficult point：Residue solution
In solid substance concentration it is high, solid particle is very thin, and size distribution is partially suspended on from less than 1 micron to a few micrometers in raffinate,
Part is in colloidal state；The presence and unconverted coal of preasphaltene and the contour glutinous object of asphaltene swelling wherein and peptization
Effect all can make viscosity very high；The alternate density contrast very little of solid-liquid two.These factors are resulted in carries out solid-liquid to coal liquefaction residue
Separating difficulty is very big, inferior separating effect, and continuous operation is difficult.
Prior art discloses a kind of separation method of coal liquefaction residue and piece-rate systems, using primary filtering, two mistakes
The mode that filter is used alternatingly, tentatively realizes continuous operation, and defect is to cause to remove since extraction mixed liquor solid content is high
Filter cake is more frequent, and filter cake uses manual cleaning, the speed of discharge rate to seriously affect continuous operation process；Discharging
Cheng Wufa seal operations, extractant are easy to volatilization pollution environment, influence operating personnel's health；And contain inside filter cake
Residual extractant can not recycle, both polluted environment, also result in the loss of extractant, increase enterprise operation cost.
Invention content
It is a primary object of the present invention to, provide a kind of good separating effect, technical process are simple, full name sealing is pollution-free,
The method and system that refined bitumen is obtained in the slave coal directly-liquefied residue of long period continuous operation can be realized, to reach coal
Liquefied residue carries out the purpose of sub-prime classified utilization.The process characteristic of this method is carried out to coal liquefaction residue using organic solvent
Extraction is separated by solid-liquid separation residue and extractant mixture by two steps, isolated refined bitumen, and it is high additional to can be used as preparation
The raw material of value carbon material prepare high performance casting coke as coking additive, and isolated extract remainder solid, which contains, not to be turned
Change coal and catalyst, can using combustion power generation, with coal gasification or as construction material.
The object of the invention to solve the technical problems is realized using following technical scheme.
A kind of pitch preparation system proposed according to the present invention, including, hybrid extraction device, the first filter element, second
Filter element, drying device and distilling apparatus, the hybrid extraction device is connected to first filter element, described
First filter element is connected to the drying device, and first filter element is connected to second filter element,
Second filter element is connected to the distilling apparatus, wherein first filter element includes at least the first mistake
Device and the second filter device are filtered, the second filter element includes at least third filter device and the 4th filter device.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, a kind of pitch preparation system above-mentioned, wherein in first filter device or the second filter device
Filter element aperture be 5-50um；Alternatively, the third filter device or the filter element in the 4th filter device
Aperture is 0.1-10um.
Preferably, a kind of pitch preparation system above-mentioned, wherein in first filter device or the second filter device
Filter element be non-woven fabrics or nylon material；Alternatively, the mistake filtering element in the third filter device or the 4th filter device
Part is stainless steel.
Preferably, a kind of pitch preparation system above-mentioned, wherein the drying device and the hybrid extraction device
Connection；Alternatively, the distilling apparatus is connected to the hybrid extraction device.
Preferably, a kind of pitch preparation system above-mentioned, wherein the drying device is pan dryer.
The object of the invention to solve the technical problems is also realized using technical solution below.
A kind of asphalt production process proposed according to the present invention, including, coal liquefaction residue and extractant are placed in described
In hybrid extraction device, stirring obtains the first mixture；First mixture is placed in first filter device
In, through the first filtering, the first filter cake and the first filtrate are obtained, first filtrate is placed in the third filter device
In, it is filtered through third, obtains the first filter residue and third filtrate, the third filtrate is distilled, pitch is obtained.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, a kind of asphalt production process above-mentioned, wherein the asphalt production process further includes that coal liquefaction is residual
Slag is placed in extractant in the hybrid extraction device, and stirring obtains the second mixture；Second mixture is placed in
In second filter device, through the second filtering, the second filter cake and the second filtrate are obtained, meanwhile, by first filter cake
The first backwash is carried out, filter powder is obtained, the filter powder is placed in drying in the drying device, obtains extractant and drying
Second filtrate is placed in the 4th filter device by object, through the 4th filtering, obtains the second filter residue and the 4th filter
Liquid, meanwhile, first filter residue is subjected to the second backwash, the 4th filtrate is distilled, pitch is obtained.
Preferably, a kind of asphalt production process above-mentioned carries out first backwash using air or inert gas,
First backwashing pressure is 0.1-1.0MPa；Alternatively, carrying out second backwash, the second backwashing pressure using extractant
For 0.2-1.2MPa.
Preferably, a kind of asphalt production process above-mentioned, wherein the filter pressure of first filtering or the second filtering
For 0.05-0.3MPa；Alternatively, the filter pressure of the third filtering or the 4th filtering is 0.1-0.6MPa.
Preferably, a kind of asphalt production process above-mentioned, wherein the extractant is toluene, tetrahydrofuran, N- methyl
The combination of one or more of pyrrolidones, petroleum ether, dimethylnaphthalene, coal liquefaction fraction oil.
By above-mentioned technical proposal, a kind of method and system preparing pitch using coal liquefaction residue provided by the invention,
At least there are following advantages：
When 1, carrying out pitch preparation using pitch preparation system provided by the invention, the type of extractant is not construed as limiting.
Different extraction items can be arranged in preparation system provided by the invention according to physical properties such as the polarity powers of extractant
Part, operation is flexible, to the adaptable of extractant；Meanwhile can different extraction items be set further according to different extractants
Part improves extraction efficiency.
2, pitch preparation system provided by the invention includes double-filtration unit, reduces DCL/Direct coal liquefaction and prepares pitch
Difficulty, obtained solid particle residual solvent levels are seldom, solve strainer existing for existing separation of solid and liquid and easily block, is fragile
The technical barrier of damage；Moreover, dual stage filter apparatus is simple in structure, floor space is small, and cost of investment is low.
The mixed liquor of coal liquefaction residue and extractant has high viscosity, solid substance concentration height, liquid phase and solid particle close
The smaller feature of degree difference causes separation of solid and liquid difficulty bigger.In pitch preparation system provided by the invention, including two-stage mistake
Unit is filtered, level-one coarse filtration is carried out using the first filter element, two level secondary filter is carried out using the second filter element, passes through two
Grade filter type is separated by solid-liquid separation, and the difficulty that coal liquefaction residue prepares pitch is reduced, and, it is remained in obtained solid particle
Quantity of solvent it is seldom, solve strainer existing in the prior art easily block, cracky the technical issues of.
And the filter apparatus configuration in filter element provided by the invention is simple, floor space is small, has saved production space,
Reduce cost of investment.
3, pitch preparation system provided by the invention realizes the continuous production that coal liquefaction residue prepares pitch.
In pitch preparation system provided by the invention, the first filter element includes at least the first filter device and the second filtering
Device, the second filter element include at least third filter device and the 4th filter device.Added when using the first filter device
While press filtration, the second filter device can be backwashed, remove the filter cake on filter element in the second filter device, it
Afterwards, while carrying out pressure filtration using the second filter device, the first filter device can be backwashed, the first filtering of removal
Filter cake in device on filter element；It, can be to the 4th filter device while carrying out pressure filtration using third filter device
It is backwashed, removes the filter residue in the 4th filter device on filter element and using the 4th filter device pressurizeed later
Filter, backwashes third filter device, removes the filter residue on filter element in third filter device.
In the preparation process of pitch, the first filter device and the second filter device in the first filter element are alternately
It filtering, the third filter device and the 4th filter device in the second filter element alternately filter, and realize continuous operation,
The production time is saved, production efficiency is improved, realizes the long-term operation of system.
4, pitch preparation system provided by the invention, whole " locked in " operation, operating process pollution-free, environmentally protective, and
Material free of losses, has farthest recycled extractant, realizes recycling for extractant.
In the mixed liquor that coal liquefaction residue is formed with extractant, solid content is very high, needs frequently multiple removal filtering production
The mode of raw filter cake, existing removal filter cake is manual cleaning, and speed is slow, has seriously affected the continuity of operation, and, discharging
Process can not carry out under air-proof condition, and extractant is easy to volatilize, and pollute environment, influence the health of operating personnel.
In system provided by the invention, for example, filter cake is detached from from filter element, is crushed using the method for backwash,
It after dusting, falls to the bottom of filter device, then powdery filter cake passes through filter device by its own gravity and kickback pressure difference
The big-diameter ball valve of bottom enters tray drying system.Processing is dried to the filter cake after dusting in tray drying system, recycling
Residual solvent, residual solvent for recycling, obtained dry solids can using combustion power generation, with coal gasification or as building
Material.
Therefore, coal liquefaction residue is carried out to the preparation of pitch using device provided by the invention, whole process is closed
Under the conditions of carry out, operating process is pollution-free.
5, using device provided by the invention carry out coal liquefaction residue arrive pitch preparation, obtained refined bitumen with compared with
High C/H atomic ratios, low ash content, low-sulfur, the feature that quinoline insolubles are relatively low, aromaticity is high, are to prepare high added value carbon
The desirable feedstock of material.
6, using device provided by the invention progress coal liquefaction residue to the preparation of pitch, obtained solid particle extract remainder
Can using combustion power generation, with coal gasification or as construction material, realize the sub-prime classification high value added utilization of liquefied residue, avoid
The waste of liquefied residue resource, the whole economic efficiency to improving liquefaction plant have very important realistic meaning.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after coordinating attached drawing to be described in detail such as.
Description of the drawings
Fig. 1 is the process flow chart of the method provided in an embodiment of the present invention that refined bitumen is obtained from coal liquefaction residue.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to a kind of method and system preparing pitch using coal liquefaction residue proposed according to the present invention,
Specific implementation mode, structure, feature and its effect are described in detail as after.In the following description, different " embodiment " or
What " embodiment " referred to is not necessarily the same embodiment.In addition, special characteristic, structure or feature in one or more embodiments can be by
Any suitable form combination.
The present invention provides a kind of pitch preparation systems, including, hybrid extraction device, the first filter element, the second filtering
Unit, drying device and distilling apparatus, the hybrid extraction device are connected to first filter element, and described first
Filter element is connected to the drying device, and first filter element is connected to second filter element, described
The second filter element be connected to the distilling apparatus, wherein first filter element include at least first filtering fill
It sets and includes at least third filter device and the 4th filter device with the second filter device, the second filter element.
The present invention provides a kind of pitch preparation systems, especially a kind of to be suitable for preparing pitch using coal liquefaction residue
Pitch preparation system.
Pitch preparation system provided by the invention includes hybrid extraction device, has agitating function, and adjustable pressure, uses
In coal liquefaction residue and extractant are mixed, stirred, is extracted, by coal liquefaction residue mink cell focus and bitumen it is molten
In solution to extractant, uniform extraction mixed liquor, i.e., the first mixture above-mentioned are formed with extractant insoluble matter.It is preferred that
, it can be by adjusting parameters such as the pressure, mixing time, mixing speed of hybrid extraction device, to be suitable for highly polar or weak pole
The different types of extractants such as property.Preferably, pitch preparation system provided by the invention further includes crusher, the crusher
For coal liquefaction residue to be crushed, it is preferred that the grain size of coal liquefaction residue is crushed to 5cm or less.
Pitch preparation system provided by the invention includes the two-stage mistake being made of the first filter element and the second filter element
Filter unit, it is preferred that level-one coarse filtration is carried out using the filter device in the first filter element, it, will after the completion of level-one coarse filtration
Filtrate is sent to secondary filtration unit, carries out two level secondary filter.
Specifically, the first mixture obtained above is pumped in the filter device of the first filter element, it is mixed to first
Object is closed to be separated by solid-liquid separation.Preferably, the mistake filtering element in the first filter device and the second filter device in the first filter element
Part is the filter cloth of oval tubular, and the undissolved big grain size solid of the major part in the first mixture is formed in filter cloth surface and is filtered
Cake contains least a portion of small particle size solid, the mink cell focus and bitumen of extractant and dissolving by the filtrate of filter cloth.It is preferred that
, filter element in first filter device or the second filter device is non-woven fabrics or nylon material, filter element
Aperture is 5-50um.The first filter device and the second filter device are included at least in first filter element provided by the invention, it is excellent
Choosing, it is connected between hybrid extraction device and the material pipeline of the first filter element, is provided with route conversion equipment, tune can be passed through
The section route conversion equipment, the first mixture of control enters the first filter device, or, into the second filter device.For example,
First mixture is entered into the first filter device, meanwhile, the filter cake in the second filter device is backwashed, by the second filtering
Filter cake removal in device, prepares for subsequent separation of solid and liquid, to realize continuous filtering.
It will be transported in the filter device of the second filter element by the filtrate of filter cloth, be further separated by solid-liquid separation,
That is, two level secondary filter.By the separation of solid and liquid of two level secondary filter process, the filtrate for being entirely free of solid and small particle are obtained
Solid matter.Preferably, the filter element in the third filter device or the 4th filter device in the second filter element is not
The aperture of rust steel material, filter element is 0.1-10um.Third is included at least in second filter element provided by the invention to filter
Device and the 4th filter device, it is preferred that between the first filter element of connection and the material pipeline of the second filter element, be provided with
Route conversion equipment, can be by adjusting the route conversion equipment, and control filtrate enter third filter device, or, into the
Four filter devices.For example, filtrate is entered into third filter device, meanwhile, the filter residue in the 4th filter device is backwashed,
It by the filter residue removal in the 4th filter device, prepares for subsequent separation of solid and liquid, to realize continuous filtering.
It will be sent into distilling apparatus by the isolated third filtrate of the second filter element or the 4th filtrate, it is preferred that
The distilling apparatus is vacuum distillation apparatus, is detached to third filtrate or the 4th filtrate using distilling apparatus, recycling extraction
Take agent for recycling, distillation tower bottom obtains the refined bitumen containing mink cell focus and bitumen.Preferably, described to subtract
Pressure distilling apparatus is made of heating furnace, destilling tower, condenser, vacuum pump etc., the connection type and operation principle be this field
The prior art known, entire decompression distillation system temperature control is within 500 DEG C.
The filter powder that backwash obtains is sent into drying device, processing is dried, recycles residual solvent, residual solvent is for following
Ring uses, obtained dry solids can using combustion power generation, with coal gasification or as construction material.Preferably, described dry
Dry device is tray drying device, and tray drying device is made of feeder, drying machine, condenser, solvent receiving tank etc., dry
Disc layer vertical.When extractant is low boiling point, high volatile solvent, drying pressure is normal pressure, and drying temperature is 50~200
℃；When extractant is higher boiling, low voc solvent, using vacuum drying mode, drying temperature is 100~300 DEG C, vacuum
Degree is 20~80kPa.
Invention further provides a kind of asphalt production process, as shown in Figure 1.
Asphalt plant above-mentioned can be used in asphalt production process provided by the invention.
When prepared by the pitch for carrying out first batch：Coal liquefaction residue and extractant are placed in the hybrid extraction device
In, stirring obtains the first mixture；First mixture is placed in first filter device, is filtered through first,
The first filter cake and the first filtrate are obtained, first filtrate is placed in the third filter device, is filtered, obtain through third
To the first filter residue and third filtrate, the third filtrate is distilled, pitch is obtained.
When prepared by the pitch for carrying out second lot：Coal liquefaction residue and extractant are placed in the hybrid extraction device
In, stirring obtains the second mixture；Second mixture is placed in second filter device, is filtered through second,
The second filter cake and the second filtrate are obtained, meanwhile, first filter cake is subjected to the first backwash, obtains filter powder, it will be described
Filter powder is placed in dry in the drying device, obtains extractant and dried object, and second filtrate is placed in described the
In four filter devices, through the 4th filtering, the second filter residue and the 4th filtrate are obtained, meanwhile, first filter residue is carried out second
Backwash, the 4th filtrate is distilled, pitch is obtained.
Asphalt production process provided by the invention can be used by the conversion of the first filter device and the second filter device,
The conversion of third filter device and the 4th filter device uses, and realizes the continuous production of pitch.
Preferably, the extractant is toluene, tetrahydrofuran, N-Methyl pyrrolidone, petroleum ether, dimethylnaphthalene, coal
Liquefy organic solvents or their mixtures such as distillate.
When extractant is intensive polar solvent such as tetrahydrofuran, N-Methyl pyrrolidone, dimethylnaphthalene equal solvent, coal liquefaction
The mass ratio of residue and extractant is 1: 2~6, preferably 1: 3, and extraction conditions is normal temperature and pressure, constant temperature mixing time is 10~
60min, preferably 20~40min, stir speed (S.S.) are 40~300r/min, preferably 50~200r/min.When extractant is first
When the weakly polar organic solvents such as benzene, dimethylbenzene, petroleum ether, coal liquefaction fraction oil, the mass ratio of coal liquefaction residue and extractant is 1
: 3~11, preferably 1: 4~8, extraction temperature be 50~200 DEG C, preferably 80~150 DEG C, constant temperature mixing time be 30~
120min, preferably 60~100min, stir speed (S.S.) are 50~500r/min, preferably 80~300r/min.
Preferably, the medium of the first backwash is pressure-air or high-pressure inert gas, the first filter device or the second mistake
The filter element for filtering device is the non-woven fabrics or nylon of tension function admirable, and the aperture of filter element element is 5~50um, filtering
Pressure is 0.05~0.3MPa；When extractant is intensive polar solvent, filtration temperature is room temperature；Extractant is weak polar solvent
When, filtration temperature is 80~150 DEG C.
It will be fallen after filter cake dusting to filter bottom by high pressure recoil, then powdery filter cake passes through its own gravity and anti-
Punching press force difference enters tray drying system by bottom big-diameter ball valve, and backwashing pressure is 0.1~1.0MPa.
Preferably, the filter element of third filter device or the 4th filter device, a diameter of 60~100mm of filter core, filter core
Aperture is 0.1~10um, preferably 0.5~2um.
As shown in Fig. 1, ground-slag and extractant of the coal liquefaction residue by crusher in crushing at granularity less than 5em press one
Certainty ratio is added to from tank top in hybrid extraction tank, and charging valve is closed after addition, is fully stirred in hybrid extraction tank
Mixing is mixed, uniform first mixture is formed.The first mixture in hybrid extraction tank enters one after feed pump is pressurized
Grade coarse filtration system (i.e. the first filter element) carries out pressure filtration, two sets of coarse filter devices of level-one coarse filtration system (i.e. first
Filter device and the second filter device) alternately filters and backwash, achieve the purpose that serialization filters.In level-one coarse filtration
For system using pressure-air or inert gas by filter cake dusting, filter cake contains remaining extractant, and extraction agent content is less than 10%,
Filter cake after dusting is sent into tray drying system by spiral inlet valve；The filtrate come out from level-one coarse filtration system is sent into two level
Ultra-filtration system (i.e. the second filter element) carries out secondary filter.Two sets of precise filtering devices of two level ultra-filtration system
(i.e. third filter device and the 4th filter device) is alternately filtered and is backwashed, using high pressure extraction agent by screen surface
After solid particle rinses, the counter-flushing liquid of formation is sent into level-one coarse filtration system and carries out coarse filtration again, with filtering time
Several increases, the concentration of solid particles in counter-flushing liquid can be higher and higher, therefore for the smooth operating of device, needs periodically
The counter-flushing liquid of high solid granule density is sent into tray drying system to be dried.It is obtained in two level ultra-filtration system
Filtrate carries out decompression distillation system and carries out vacuum distillation recycling extractant, and extractant recycles；Distillation tower bottom is refined
Asphaltic products.In tray drying system, the filter cake containing residual extractant is dried, the extractant being dried to obtain is followed
Ring utilizes, the dry cake that tray drying bottom of device obtains i.e. extract remainder can using combustion power generation, with coal gasification or as building
Material.
Embodiment 1
200kg coal liquefaction residues are crushed as particle diameter in 1cm residue powder below, with 500kg tetrahydrofuran solvents
Carry out being sufficiently mixed stirring under normal temperature condition in hybrid extraction tank, stirring obtains uniform mixture after 30 minutes, then into
Row level-one coarse filtration, filtration temperature are room temperature, and filter cloth aperture is 10um, and filter pressure 0.2MPa uses N2It recoils, recoils
It is 150 DEG C that filter cake after dusting, which is sent into tray drying system disc type drying device drying temperature, obtains the drying without extractant
Extract remainder.
The filtrate obtained from level-one coarse filtration system enters two level ultra-filtration system, aperture of filter screen 1um, filter pressure
It for 0.4MPa, is recoiled to the small particle size solid on strainer with extractant, kickback pressure 0.9MPa, counter-flushing liquid is sent into one
Grade coarse filtration system is filtered again.
The filtrate obtained from two level ultra-filtration system is sent into decompression distillation system and carries out solvent recovery, vacuum distillation temperature
It it is 200 DEG C, the serious reciprocal of duty cycle of destilling tower is 30kPa, and the extractant distilled recycles, and destilling tower bottom obtains refined bitumen production
Product.
The property of coal liquefaction residue is shown in Table 1, and the specific test result of embodiment 1 is as shown in table 2.
Embodiment 2
100kg coal liquefaction residues are crushed as particle diameter in 5mm residue powder below, with matter oil in 600kg coal liquefactions
(boiling range is 200~260 DEG C) carries out being sufficiently mixed stirring in hybrid extraction tank, after being stirred 100 minutes under the conditions of 80 DEG C
To uniform mixture, level-one coarse filtration is then carried out, filtration temperature is room temperature, and filter cloth aperture is 5um, and filter pressure is
0.3MPa is recoiled with air, and the filter cake after the dusting that recoils is sent into tray drying system, and tray drying device drying temperature is
300 DEG C, obtain the drying extract remainder without extractant.
The filtrate obtained from level-one coarse filtration system enters two level ultra-filtration system, aperture of filter screen 1um, filter pressure
It for 0.5MPa, is recoiled to the small particle size solid on strainer with extractant, kickback pressure 0.8MPa, counter-flushing liquid is sent into one
Grade coarse filtration system is filtered again.
The filtrate obtained from two level ultra-filtration system is sent into decompression distillation system and carries out solvent recovery, vacuum distillation temperature
It it is 400 DEG C, the serious reciprocal of duty cycle of destilling tower is 20kPa, and the extractant distilled recycles, and destilling tower bottom obtains refined bitumen production
Product.
The property of coal liquefaction residue is shown in Table 1, and the specific test result of embodiment 2 is as shown in table 2.
Embodiment 3
100kg coal liquefaction residues are crushed as particle diameter in 1cm residue powder below, are mixed with 400kg mixed solvents,
Mixed solvent type is toluene, tetrahydrofuran, petroleum ether, and mass ratio is respectively 50%, 20%, 30%, mixed solvent and coal liquid
To change residue to carry out being sufficiently mixed stirring under normal temperature condition in hybrid extraction tank, stirring obtains uniform mixture after sixty minutes,
Then level-one coarse filtration is carried out, filtration temperature is room temperature, and filter cloth aperture is 5um, and filter pressure 0.3MPa uses N2It carries out anti-
Punching, the filter cake after the dusting that recoils are sent into tray drying system, and tray drying device drying temperature is 250 DEG C, is obtained without extraction
The drying extract remainder of agent.
The filtrate obtained from level-one coarse filtration system enters two level ultra-filtration system, aperture of filter screen 0.5um, filtration pressure
Power is 0.5MPa, is recoiled to the small particle size solid on strainer with extractant, kickback pressure 0.8MPa, and counter-flushing liquid is sent into
Level-one coarse filtration system is filtered again.
The filtrate obtained from two level ultra-filtration system is sent into decompression distillation system and carries out solvent recovery, decompression distillation system
Temperature is 400 DEG C, and the serious reciprocal of duty cycle of destilling tower is 30kPa, and the extractant distilled recycles, and destilling tower bottom obtains refined drip
Green product.
The property of coal liquefaction residue is shown in Table 1, and the specific test result of embodiment 3 is as shown in table 2.
1 coal directly-liquefied residue property of table
The specific test result of 2 embodiment 1-3 of table
Remarks：1. extraction yield=(mink cell focus and asphalt mixture weight/coal liquefaction residue weight) × 100
2. solvent recovering rate=(recycling design weight/extractant weight) × 100
The method and system provided by the invention that refined bitumen is obtained from coal liquefaction residue are can be seen that from the data of table 2
Extraction yield is high, substantially by coal liquefaction residue mink cell focus and bitumen all extract, solvent recovering rate is high, drop
Low operating cost；Refined bitumen has that higher C/H atomic ratios, low ash content, low-sulfur, quinoline insolubles be relatively low, aromaticity
High feature is the desirable feedstock for preparing high added value carbon materials.
In the above-described embodiments, it all emphasizes particularly on different fields to the description of each embodiment, there is no the portion being described in detail in some embodiment
Point, it may refer to the associated description of other embodiment.
It is understood that the correlated characteristic in above-mentioned apparatus can be referred to mutually.In addition, in above-described embodiment " the
One ", " second " etc. is and not represent the quality of each embodiment for distinguishing each embodiment.
In the instructions provided here, numerous specific details are set forth.It is to be appreciated, however, that the implementation of the present invention
Example can be put into practice without these specific details.In some instances, well known structure and skill is not been shown in detail
Art, so as not to obscure the understanding of this description.
Similarly, it should be understood that in order to simplify the disclosure and help to understand one or more of each inventive aspect,
Above in the description of exemplary embodiment of the present invention, each feature of the invention is grouped together into single implementation sometimes
In example, figure or descriptions thereof.However, the device of the disclosure should be construed to reflect following intention：It is i.e. required to protect
Shield the present invention claims the more features of feature than being expressly recited in each claim.More precisely, as following
Claims reflect as, inventive aspect is all features less than single embodiment disclosed above.Therefore,
Thus the claims for following specific implementation mode are expressly incorporated in the specific implementation mode, wherein each claim itself
All as a separate embodiment of the present invention.
Heretofore described numberical range includes numerical value all within the scope of this, and includes any two within the scope of this
The value range of numerical value composition.
Technical characteristic in the claims in the present invention and/or specification can be combined, and a combination thereof mode is not limited to weigh
The combination that profit is obtained in requiring by adduction relationship.It is combined by the technical characteristic in claim and/or specification
The technical solution and protection scope of the present invention arrived.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to the technical spirit of the present invention to any simple modification, equivalent change and modification made by above example, this hair is still fallen within
In the range of bright technical solution.
Claims (10)
1. a kind of pitch preparation system, it is characterised in that：Including,
Hybrid extraction device, the first filter element, the second filter element, drying device and distilling apparatus,
The hybrid extraction device is connected to first filter element, first filter element and the drying
Device is connected to, and first filter element is connected to second filter element, second filter element with it is described
Distilling apparatus connection,
Wherein, first filter element includes at least the first filter device and the second filter device,
Second filter element includes at least third filter device and the 4th filter device.
2. a kind of pitch preparation system according to claim 1, it is characterised in that：
Filter element in first filter device or the second filter device is non-woven fabrics or nylon material；
Alternatively,
Filter element in the third filter device or the 4th filter device is stainless steel.
3. a kind of pitch preparation system according to claim 1, it is characterised in that：
The aperture of first filter device or the filter element in the second filter device is 5-50um；
Alternatively,
The aperture of the third filter device or the filter element in the 4th filter device is 0.1-10um.
4. a kind of pitch preparation system according to claim 1, it is characterised in that：
The drying device is connected to the hybrid extraction device；Alternatively,
The distilling apparatus is connected to the hybrid extraction device.
5. a kind of pitch preparation system according to claim 1, it is characterised in that：
The drying device is pan dryer.
6. a kind of asphalt production process, it is characterised in that：
Using the system described in any one of claim 1-5, preparation method includes,
Coal liquefaction residue and extractant are placed in the hybrid extraction device, stirring obtains the first mixture；
First mixture is placed in first filter device, through the first filtering, obtains the first filter cake and first
Filtrate,
First filtrate is placed in the third filter device, is filtered through third, obtains the first filter residue and third filter
Liquid,
The third filtrate is distilled, pitch is obtained.
7. a kind of asphalt production process according to claim 6, it is characterised in that：Further include,
Coal liquefaction residue and extractant are placed in the hybrid extraction device, stirring obtains the second mixture；
Second mixture is placed in second filter device, through the second filtering, obtains the second filter cake and second
Filtrate, meanwhile, first filter cake is subjected to the first backwash, filter powder is obtained, the filter powder is placed in the drying
It is dry in device, extractant and dried object are obtained,
Second filtrate is placed in the 4th filter device, through the 4th filtering, obtains the second filter residue and the 4th filter
Liquid, meanwhile, first filter residue is subjected to the second backwash,
4th filtrate is distilled, pitch is obtained.
8. a kind of asphalt production process according to claim 7, it is characterised in that：
First backwash is carried out using air or inert gas, the first backwashing pressure is 0.1-1.0MPa；
Alternatively,
Second backwash is carried out using extractant, the second backwashing pressure is 0.2-1.2MPa.
9. a kind of asphalt production process according to claim 7, it is characterised in that：
The filter pressure of first filtering or the second filtering is 0.05-0.3MPa；
Alternatively,
The filter pressure of the third filtering or the 4th filtering is 0.1-0.6MPa.
10. a kind of asphalt production process according to claim 6, it is characterised in that：
The extractant is in toluene, tetrahydrofuran, N-Methyl pyrrolidone, petroleum ether, dimethylnaphthalene, coal liquefaction fraction oil
A combination of one or more.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181730A (en) * | 2018-09-30 | 2019-01-11 | 中国科学院山西煤炭化学研究所 | A kind of kerosene refines the method that residue prepares needle coke altogether |
| CN109401776A (en) * | 2018-09-30 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A kind of method and device of asphalt high-temperature extraction heat |
| CN111218294A (en) * | 2018-11-27 | 2020-06-02 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
| CN113025366A (en) * | 2019-12-24 | 2021-06-25 | 国家能源投资集团有限责任公司 | System and method for treating direct coal liquefaction residues |
| CN113025364A (en) * | 2019-12-24 | 2021-06-25 | 国家能源投资集团有限责任公司 | System and method for treating direct coal liquefaction residues |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07305072A (en) * | 1994-05-12 | 1995-11-21 | Nippon Steel Corp | Method for both taking out liquefaction residue in coal liquefying process and recovering coal liquefying catalyst |
| 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 |
| CN103242881A (en) * | 2013-05-30 | 2013-08-14 | 神华集团有限责任公司 | Method for separating bituminous substances from coal direct liquefaction residues |
| CN103613089A (en) * | 2013-11-29 | 2014-03-05 | 神华集团有限责任公司 | Method of preparing mesocarbon microbeads by coal liquefaction residues and mesocarbon microbeads |
| CN103614153A (en) * | 2013-11-29 | 2014-03-05 | 神华集团有限责任公司 | Preparation method of polycondensed asphalt, preparation method of needle coke and needle coke |
| CN105087058A (en) * | 2015-08-04 | 2015-11-25 | 煤炭科学技术研究院有限公司 | Separation method and system for coal liquefaction residues |
-
2018
- 2018-03-14 CN CN201810212523.0A patent/CN108410491A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07305072A (en) * | 1994-05-12 | 1995-11-21 | Nippon Steel Corp | Method for both taking out liquefaction residue in coal liquefying process and recovering coal liquefying catalyst |
| 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 |
| CN103242881A (en) * | 2013-05-30 | 2013-08-14 | 神华集团有限责任公司 | Method for separating bituminous substances from coal direct liquefaction residues |
| CN103613089A (en) * | 2013-11-29 | 2014-03-05 | 神华集团有限责任公司 | Method of preparing mesocarbon microbeads by coal liquefaction residues and mesocarbon microbeads |
| CN103614153A (en) * | 2013-11-29 | 2014-03-05 | 神华集团有限责任公司 | Preparation method of polycondensed asphalt, preparation method of needle coke and needle coke |
| CN105087058A (en) * | 2015-08-04 | 2015-11-25 | 煤炭科学技术研究院有限公司 | Separation method and system for coal liquefaction residues |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181730A (en) * | 2018-09-30 | 2019-01-11 | 中国科学院山西煤炭化学研究所 | A kind of kerosene refines the method that residue prepares needle coke altogether |
| CN109401776A (en) * | 2018-09-30 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A kind of method and device of asphalt high-temperature extraction heat |
| CN109401776B (en) * | 2018-09-30 | 2020-12-01 | 中国科学院山西煤炭化学研究所 | Method and device for high-temperature thermal extraction of asphalt |
| CN111218294A (en) * | 2018-11-27 | 2020-06-02 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
| CN111218294B (en) * | 2018-11-27 | 2021-07-23 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
| CN113025366A (en) * | 2019-12-24 | 2021-06-25 | 国家能源投资集团有限责任公司 | System and method for treating direct coal liquefaction residues |
| CN113025364A (en) * | 2019-12-24 | 2021-06-25 | 国家能源投资集团有限责任公司 | System and method for treating direct coal liquefaction residues |
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Application publication date: 20180817 |