CN106978203A - A kind of coal tar takes off slag and fraction seperation technique and device - Google Patents
A kind of coal tar takes off slag and fraction seperation technique and device Download PDFInfo
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- CN106978203A CN106978203A CN201710237562.1A CN201710237562A CN106978203A CN 106978203 A CN106978203 A CN 106978203A CN 201710237562 A CN201710237562 A CN 201710237562A CN 106978203 A CN106978203 A CN 106978203A
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- coal tar
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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
- C10C1/00—Working-up tar
- C10C1/18—Working-up tar by extraction with selective solvents
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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
- C10C1/00—Working-up tar
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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
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
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- Oil, Petroleum & Natural Gas (AREA)
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- Working-Up Tar And Pitch (AREA)
Abstract
A kind of coal tar takes off slag and fraction seperation technique and device, mixed, extracted with coal tar using solvent in coal tar extractive reaction kettle, then isolated tar slag and solvent extract are carried out in solid-liquid separator, slag is further taken off by vacuum flasher and filter；Solvent extract enters the first decompression vaporizer and obtains solvent and de- dross coal tar, and solvent reusable edible through the condensation of the first condensing unit；De- dross coal tar enters the second decompression vaporizer and obtains coal tar heavy component and coal tar light components through the condensation of the second condensing unit.Slag and fraction seperation technique and device are taken off it is an object of the invention to provide a kind of coal tar, and the technique can realize that effective fractionation, low process energy consumption, non-wastewater discharge, the equipment investment of coal tar oil ingredient be few, continuous production is easily enlarged production scale.
Description
Technical field
The invention belongs to technical field of coal chemical industry, it is related to a kind of coal tar and takes off slag and fraction seperation technique and device.
Background technology
With rapid economic development, China has turned into world energy sources and has consumed big country, market to the demand of oil product increasingly
Increase, oil supply deficiency is outstanding day by day, seeks new alternative energy source imperative.China possesses the coal resources of relative abundance
With large quantities of coal chemical enterprises, a large amount of coal tar of by-product.The coal tar obtained from the dry distillation of coal and pyrolysis is very valuable industrial chemicals,
The almost all of carbazole of in the market and quinoline all derive from coal tar, and most of anthracene, acenaphthene and pyrene are also to be passed through from coal tar
Processing, separation, extraction are obtained.As can be seen here, coai-tar product world's industrial chemicals this part in occupation of and its it is important
Status.
Coal-tar residue is a kind of poisonous and hazardous waste residue, deals with improperly and easily causes environmental pollution, and coal-tar residue is in high temperature
It is lower easily to occur coking, block pipeline, have a certain degree of influence on process equipment and catalyst etc., so in coal tar pretreatment
It is vital that slag is taken off in stage.Current coal tar, which takes off slag technology, to be had：Solvent extraction and separation, emchanically centrifugal separation, pyrolysis point
From etc..During using emchanically centrifugal separation technology, because the coal-tar residue constituent difference of separate sources is larger, to adapt to centrifugation
The performance of machine, generally requires and is further processed after coal-tar residue is pre-processed or is centrifuged, with operating
Journey is cumbersome, the shortcomings of cost of equipment is high.Coal Tars separation method is adaptable to coal-tar residue composition, hardly
Secondary pollution is caused, but it is higher to consume energy.
Coal tar as Coal dressing important by-products, by separated can obtain light oil distillate, carbolic oil cut,
Fraction of naphthalene oil, wash oil fraction, carbolineum cut and pitch, neutral component can be obtained by carrying out chemical treatment for first five kind cut
(benzene,toluene,xylene, naphthalene, anthracene etc.), acidic components (phenol, cresols, naphthols etc.) and basic component (picoline, naphthylamines,
Quinoline etc.).By these components carry out deep processing, obtained product be widely used in plastics, coating, synthetic fibers, synthetic rubber,
The fields such as medicine, agricultural chemicals, fine chemistry industry and exotic material.
Describe a kind of coal tar electro-desalting, dehydration, the method for de- slag in Chinese patent CN103102933A, this method from
Sodium carbonate liquor is added in pending coal tar, is sufficiently mixed and the heating that exchanges heat, by coal tar after the sodium salt of stabilization to be formed
The filtering of mechanical admixture twice is carried out, the coal tar after filtering is continued to heat up, and water filling and demulsifier are carried out on pipeline, is passed through
After static mixer mixing, electro-desalting, dehydration equipment are finally entered, desalination, dehydration are carried out in the presence of high voltage electric field, is taken off
Slag.The complex operation, de- slag efficiency is low, and energy consumption is higher, is not easy to expand the scale of production.
A kind of coal tar deep processing preprocess method is described in Chinese patent CN105316018A, the present invention is using centrifugation
Separation, gas back-flushing filtering, distillation, high voltage electric field carry out de- slag, deamination water, dephenolize, desalination to coal tar respectively, in being adapted to
The pretreatment of low temperature or high temperature coal-tar, but process low separation efficiency, complex operation, the high energy consumption.
A kind of dry distillation of coal and coal tar distillation combined technical method, feed coal are described in Chinese patent CN105647554A
The coal tar heavy end that powder is isolated with Distallation systm enters microwave treatment reaction after being sufficiently mixed in the solid mixing apparatus of liquid
Device generation coal gas, semicoke and coal tar；Coal tar is separated into coal tar light fraction, coal tar into Distallation systm after pretreatment
Oily heavy end and coal tar asphalt, coal tar heavy end are recycled back to the solid mixing apparatus of liquid and mixed with coal dust.Coal in this method
It is low that tar distillation cuts cut efficiency, separates not thorough, and the narrower cut of temperature range is difficult cutting.
A kind of efficient fractionating device, including fractionation room, heater, temperature are described in Chinese patent CN205516583U
Induction installation, gas outlet, bridge piece, connecting tube, parameter display screen, visual window, fluid reservoir air inlet pipe, fluid reservoir, cooling storehouse
Deng.Though the fractionating device can understand the running situation of equipment in time, structure is excessively complicated, cumbersome, is unfavorable for extensive
Production.
In summary, not only energy consumption is big for the de- slag of traditional coal tar and fraction seperation technique, various waste water is produced, to environment
A certain degree of pollution is caused, and separative efficiency is relatively low, separates not thorough, complex operation, it is time-consuming.So, searching is pollution-free,
Low energy consumption, a kind of efficient coal tar take off slag and fraction seperation technology tool has very important significance.
The content of the invention
In order to overcome problem present in currently available technology, take off slag it is an object of the invention to provide a kind of coal tar and evaporate
Divide separating technology and device, the technique can realize effective fractionation, low process energy consumption, non-wastewater discharge, the operation of coal tar oil ingredient
Simply it is easily enlarged production scale.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of coal tar takes off slag and fraction seperation device, including dehydrated coal tar storage tank, coal tar extractive reaction kettle, solvent
Storage tank, solvent extract storage tank, the first tubular preheater, the first decompression vaporizer, the second tubular preheater and the second decompression
Vaporizer；
Dehydrated coal tar storage tank is connected with coal tar extractive reaction kettle top entry, and coal tar extractive reaction bottom portion goes out
Mouth is connected with solid-liquid separator top entry, and solid-liquid separator outlet at bottom is connected with solvent extract charging pump intake, molten
Agent extract feed pump discharge is connected through voltage transformation controller with two filters, each filter with tar slag storage tank and
Solvent extract storage tank is connected；
Solvent tank outlet is divided into two-way, is connected all the way with coal tar extractive reaction kettle top entry, and another road is with becoming
Pressure controller is connected；
Solvent extract outlet is connected with the first tubular preheater entrance, and the outlet of the first tubular preheater subtracts with first
Pressure chamber input is connected, and the first decompression bottom of vaporizing chamber outlet is connected with the second tubular preheater entrance, and the second tubular type is pre-
Hot device outlet is connected with the second decompression chamber input, and the second decompression vaporizer top exit is connected with the second condensing unit.
Further improve of the invention is that two filters include the first filter, the second filter, voltage transformation controller
It is connected with the first filter, the second filter top entrance, the outlet at bottom of the first filter is divided into two-way, all the way with tar
Slag storage tank is connected, and another road is connected with solvent extract storage tank；The outlet of second filter bottom is divided into two-way, all the way with Jiao
Dregs of fat storage tank is connected, and another road is connected with solvent extract storage tank.
Further improve of the invention is, the first rotary sprayer, the second filtering are provided with the first filter inlet
Device porch is provided with the second rotary sprayer, and being provided with the 3rd rotary sprayer second at the first decompression chamber input depressurizes
The 4th rotary sprayer is provided with chamber input.
Further improve of the invention is that solid-liquid separator outlet at bottom is also connected with vacuum flasher top entry
Logical, the condensed device of side outlet is connected with solvent extract charging pump intake on vacuum flasher, vacuum flasher outlet at bottom
It is connected with tar slag storage tank.
Further improve of the invention is that the first decompression vaporizer top exit is connected with the first condensing unit entrance
Logical, the first condensing unit outlet at bottom is connected with solvent tank.
Further improve of the invention is that the first decompression bottom of vaporizing chamber outlet is through de- dross coal tar storage tank and the second pipe
Formula pre-heater inlet is connected；Dehydrated coal tar storage tank, solvent tank, tar slag storage tank, solvent extract storage tank, de- dross coal tar
Storage tank, coal tar heavy component storage tank and coal tar light components tank inside are provided with liquid level gauge.
The present invention, which is further improved, to be, the second condensing unit outlet at bottom and coal tar light components reservoir inlet phase
Connection；Second decompression bottom of vaporizing chamber outlet is connected with coal tar heavy component reservoir inlet.
A kind of coal tar takes off slag and fraction seperation technique, comprises the following steps：
1) coal tar takes off slag technological process
Injected after dehydrated coal tar is preheated in coal tar extractive reaction kettle, while solvent is heated and pressurizeed by solvent tank
After be pumped into coal tar extractive reaction kettle；In coal tar extractive reaction kettle after heating, extraction, solvent is mixed with dehydrated coal tar
Compound is separated through solid-liquid separator, obtains tar slag and solvent extract；
Solvent extract is added in the first filter through the first rotating spraying and filtered, and filtrate enters solvent extract
Storage tank；When the pressure of the first filter interior reaches setting value, the second filter is automatically switched to by voltage transformation controller and carried out
Filtering, is passed through solvent and the filter screen in the first filter is cleaned, when the second vacuum filter internal pressure reaches setting value
When, the first filter is automatically switched to by voltage transformation controller and filtered, and it is clear to the progress of the second vacuum filter to be passed through solvent
Wash；The first vacuum filter is set mutually to switch with the second vacuum filter by voltage transformation controller；
2) coal tar fraction separating technology flow
Solvent extract storage tank internal solvent extract is added in the first tubular preheater, first is sprayed at after preheating and is subtracted
In pressure vaporizer, solvent vapo(u)r enters in the first condensing unit at the top of the first decompression vaporizer, condensed rear inflow solvent tank
In, is pumped into after de- dross coal tar pressurization obtained by the first decompression bottom of vaporizing chamber in the second tubular preheater, the is sprayed at after preheating
In two decompression vaporizers, light component is light into coal tar after being condensed into the second condensing unit at the top of the second decompression vaporizer
In matter component storage tank, coal tar heavy component obtained by the second decompression bottom of vaporizing chamber enters in coal tar heavy component storage tank.
Further improve of the invention is that solvent is tetrahydrofuran, dichloromethane or toluene；First tubular preheater is pre-
The temperature of hot solvent extract is 40~100 DEG C；The first decompression vaporizer internal upper part sets column plate, and the number of plates is 5~8
Block, pressure limit 1kPa~0.09MPa；The temperature of the de- dross coal tar of second tubular preheater preheating is 100~600 DEG C；Second
Depressurize vaporizer internal upper part and column plate is set, the number of plates is 8~12 pieces, pressure limit 1kPa~0.09MPa；Coal tar extractive reaction
Dehydrated coal tar and solvent volume ratio are 1 in kettle：(0.5~2).
Further improve of the invention is that the filter screen is acidproof corrosion resistant braid fabric or ceramic filter screen, hole
Footpath is 25~75um；First rotary sprayer, the second rotary sprayer, the 3rd rotary sprayer and the 4th rotary sprayer
Gun slot be 75~100um；The rotating speed of first rotary sprayer and second turn of rotary sprayer is 10~100r/min；The
The rotating speed of three rotary sprayers and the 4th turn of rotary sprayer is 10~50r/min.
Compared with prior art, the device have the advantages that：The present invention is adopted by setting coal tar extractive reaction kettle
Extracted, separated by solid-liquid separator, Ran Hou in coal tar extractive reaction kettle with dehydrated coal tar with solvent
Two filters further remove the gred, and carry out removing solvent through the first decompression vaporizer, then carry out coal tar through the second decompression vaporizer
Component fractionation, obtains coal tar heavy component and coal tar light components.Present apparatus occupation of land is small, and simple in construction, cost is low, it is easy to
Industrialization is realized, solvent can be recycled, waste water not produced environment be polluted, and can realize that coal tar takes off slag and evaporated
Divide separating technology continuous operation.
Further, by setting vacuum flasher, solvent extract in tar slag can be made further to be separated.
Further, by setting the first filter and the second filter, the first mistake is enabled to using voltage transformation controller
Filter and the second filter mutually switch automatically, de- slag technique is realized continuous operation.
Further, by setting the first rotary sprayer, the second rotary sprayer, the 3rd rotary sprayer, the 4th rotation
Turning sprayer makes coal tar and its mixture be disperseed well.
Dehydrated coal tar, solvent are added in coal tar extractive reaction kettle by the present invention, in coal tar extractive reaction kettle
After heating, extraction, solvent is separated with dehydrated coal tar mixture through solid-liquid separator, tar slag and solvent extraction is tentatively obtained
Thing；Tar slag addition vacuum flasher is further obtained into tar slag component and solvent extract, by solvent extract through first
Filter, the second filter are further filtrated to get tar slag component and solvent extract；Gained solvent extract is added to
After the preheating of first tubular preheater, entering the vaporization of the first decompression vaporizer makes solvent be separated with coal tar, solvent vapo(u)r
Into the condensation of the first condensing unit, solvent is obtained, de- dross coal tar is obtained in the first decompression bottom of vaporizing chamber；By de- dross coal tar
It is added to after the preheating of the second tubular preheater, entering the vaporization of the second decompression vaporizer is separated coal tar oil ingredient, lightweight
Component is condensed into the second condensing unit, obtains coal tar light components, and coal tar heavy duty is obtained in the second decompression bottom of vaporizing chamber
Matter component；The present invention can realize that coal tar takes off the continuous operation of slag technique and the continuous separation of cut, obtain coal tar heavy group
Divide and coal tar light components.With effective fractionation, low process energy consumption, non-wastewater discharge, equipment investment be few, continuous production is easy
In the advantage expanded the scale of production, overcome coal tar in the prior art take off energy consumption present in slag and fraction seperation process it is big,
Multi-process handling and complicated, product each component fractionation, the problem of environmental pollution is serious.The present invention is green fractionation process, extraction
Agent is recycled, and the operating condition of technique is gentle, easy, and technique and equipment manufacturing cost are low.
Further, the first rotary sprayer, the second rotary sprayer, the 3rd rotary sprayer and the 4th rotating spraying
Device can be such that coal oil mixture uniformly sprays.
Brief description of the drawings
Fig. 1 takes off slag technological process for the coal tar of the present invention；
Fig. 2 is coal tar fraction separating technology flow of the invention；
Fig. 3 is the total ion chromatogram of light 1 component of middle coalite tar；
Fig. 4 schemes for the TG of light 1 component of middle coalite tar；
Fig. 5 is the total ion chromatogram that middle coalite tar weighs 1 component；
Fig. 6 is the TG figures that middle coalite tar weighs 1 component；
Fig. 7 is the total ion chromatogram of light 2 component of middle coalite tar；
Fig. 8 schemes for the TG of light 2 component of middle coalite tar；
Fig. 9 is the total ion chromatogram that middle coalite tar weighs 2 components；
Figure 10 is the TG figures that middle coalite tar weighs 2 components；
In figure, 1, dehydrated coal tar storage tank；2nd, solvent tank；3rd, the first valve；4th, solvent feed pump；5th, the second valve；
6th, coal tar extractive reaction kettle；7th, solid-liquid separator；8th, vacuum flasher；9th, condenser；10th, tar slag storage tank；11st, solvent extracts
Take thing feed pump；12nd, the 3rd valve；13rd, voltage transformation controller；14th, the first rotary sprayer；15th, the first filter；16th, second
Rotary sprayer；17th, the second filter；18th, solvent extract storage tank；19th, the 4th valve；20th, the first tubular preheater；21、
3rd rotary sprayer；22nd, the first decompression vaporizer；23rd, the first condensing unit；24th, dross coal tar storage tank is taken off；25th, dross coal is taken off
Tar feed pump；26th, the 5th valve；27th, the second tubular preheater；28th, the 4th rotary sprayer；29th, the second decompression vaporizer；
30th, coal tar heavy component storage tank；31st, the second condensing unit；32nd, coal tar light components storage tank.
Embodiment
The present invention is described in further detail by embodiment below in conjunction with accompanying drawing.
Dehydrated coal tar storage tank 1, solvent tank 2, tar slag storage tank 10, solvent extract storage tank 18, de- slag in the present invention
Liquid level gauge is both provided with inside coal tar oil tank 24, coal tar heavy component storage tank 30 and coal tar light components storage tank 32；
Dehydrated coal tar storage tank 1, solvent tank 2, coal tar extractive reaction kettle 6, vacuum flasher 8, the filtering of the first filter 15, second
Device 17, the first tubular preheater 20, the second tubular preheater 27, first decompression decompression equal band of vaporizer 29 of vaporizer 22, second
There is the specific preheating temperature of solvent in heating mantle, the present invention, can be set according to specific solvent.
Dehydrated coal tar storage tank 1, coal tar extractive reaction kettle 6, solid-liquid separator 7, vacuum flasher 8；Solvent extract
Storage tank 18, the first tubular preheater 20, first decompression vaporizer 22, the first condensing unit 23；De- dross coal tar 24, the second tubular type
The decompression of preheater 27, second vaporizer 29, the second condensing unit 31 are cascaded structures；First filter 15 and second is filtered
Device 17 is parallel-connection structure.
Dehydrated coal tar is middle low temperature or high temperature coal-tar dehydration gained in the present invention.
Referring to Fig. 1 and Fig. 2, a kind of coal tar, which takes off slag and fraction seperation device, to be included：Dehydrated coal tar storage tank 1, solvent storage
Tank 2, the first valve 3, solvent feed pump 4, the second valve 5, coal tar extractive reaction kettle 6, solid-liquid separator 7, vacuum flasher
8th, condenser 9, tar slag storage tank 10, solvent extract feed pump 11, the 3rd valve 12, voltage transformation controller 13, the first rotation spray
Day with fog 14, the first filter 15, the second rotary sprayer 16, the second filter 17, solvent extract storage tank 18, the 4th valve
19th, the first tubular preheater 20, the 3rd rotary sprayer 21, first decompression vaporizer 22, the first condensing unit 23, de- dross coal are burnt
Oil tank 24, de- dross coal tar feed pump 25, the 5th valve 26, the second tubular preheater 27, the 4th rotary sprayer 28, second
Depressurize vaporizer 29, coal tar heavy component storage tank 30, the second condensing unit 31 and coal tar light components storage tank 32.
Referring to Fig. 1, dehydrated coal tar storage tank 1 is connected through the first valve 3 with the top entry of coal tar extractive reaction kettle 6,
The outlet at bottom of coal tar extractive reaction kettle 6 is connected with the top entry of solid-liquid separator 7, and the outlet at bottom of solid-liquid separator 7 is divided into
Two-way, is connected with the top entry of vacuum flasher 8 all the way, the condensed device 9 of side outlet and solvent extract on vacuum flasher 8
The entrance of feed pump 11 is connected；The outlet at bottom of vacuum flasher 8 is connected with tar slag storage tank 10；Another road and solvent extract
The entrance of feed pump 11 is connected, and solvent extract feed pump 11 is exported through the 3rd valve 12, the filter of voltage transformation controller 13 and first
15th, the top entry of the second filter 17 is connected, and the outlet at bottom of the first filter 15 is divided into two-way, all the way with tar slag storage tank
10 are connected, and another road is connected with solvent extract storage tank 18；Likewise, the outlet at bottom of the second filter 17 is divided into two-way,
It is connected all the way with tar slag storage tank 10, another road is connected with solvent extract storage tank 18.
The outlet of solvent tank 2 is connected with the entrance of solvent feed pump 4, and the outlet of solvent feed pump 4 is divided into two-way, all the way with coal tar
The oily top entry of extractive reaction kettle 6 is connected, another the second valve of road 5, the filter 15, second of voltage transformation controller 13 and first
The top entry of filter 17 is connected.
Referring to Fig. 2, solvent extract storage tank 18 is exported to be connected through the 4th valve 19 with the entrance of the first tubular preheater 20, the
One tubular preheater 20 is exported to be connected with the first decompression entrance of vaporizer 22, the first decompression top exit of vaporizer 22 and first
The entrance of condensing unit 23 is connected, and the outlet at bottom of the first condensing unit 23 is connected with solvent tank 2；First decompression vaporizer 22 bottom
Portion outlet is connected with taking off the entrance of dross coal tar storage tank 24, takes off dross coal tar storage tank 24 and exports warp and takes off dross coal tar feed pump 25, the
Five valves 26 are connected with the entrance of the second tubular preheater 27, the outlet of the second tubular preheater 27 and the second decompression entrance of vaporizer 29
It is connected, the second decompression top exit of vaporizer 29 is connected with the second condensing unit 31, the outlet at bottom of the second condensing unit 31 and coal
The entrance of tar light components storage tank 32 is connected；The second decompression outlet at bottom of vaporizer 29 and coal tar heavy component storage tank 30
Entrance is connected.
First rotary sprayer 14 is arranged on the porch of the first filter 15, and the second rotary sprayer 16 is arranged on the second mistake
The porch of filter 17, the 3rd rotary sprayer 21 is arranged on the porch of the first decompression vaporizer 22, and the 4th rotary sprayer 28 is set
Put in the second decompression vaporizer 29 porch.
The coal tar of the present invention takes off slag and fraction seperation technique comprises the following steps：
First, coal tar takes off slag technological process
Referring to Fig. 1, dehydrated coal tar is preheating to after 40 DEG C~100 DEG C and injected in coal tar extractive reaction kettle, while molten
Agent (tetrahydrofuran, dichloromethane or toluene) by solvent tank 2 be heated to 40 DEG C~100 DEG C after be forced into through solvent feed pump 4
It is pumped into after 0.2~0.5MPa in coal tar extractive reaction kettle 6；Dehydrated coal tar and solvent volume in coal tar extractive reaction kettle 6
Than for 1：(0.5~2)；
In coal tar extractive reaction kettle 6 after heating, extraction, by solvent and dehydrated coal tar mixture through solid-liquid separator
7 separation, tentatively obtain tar slag and solvent extract, tar slag further obtains tar slag and solvent into vacuum flasher 8
Extract.
Through the isolated solvent extract of solid-liquid separator 7 and the isolated solvent extract of vacuum flasher 8
It is homogeneously added into the first filter 15 and is filtered through the first rotating spraying 14, filtrate enters solvent extract storage tank 18；
When pressure inside the first filter 15 reaches setting value (1kPa~0.09MPa), voltage transformation controller 13 automatically switches to
Tow filtrator 17 is filtered, and is passed through solvent (tetrahydrofuran, dichloromethane or toluene) and the filter screen in the first filter 15 is entered
Row elution, leacheate enters solvent extract storage tank 18, filter screen is overturn, and is passed through the filter residue on nitrogen purging filter screen, filter
Slag is stored in tar slag storage tank 10, is again overturn filter screen after purging is clean；When the internal pressure of the second vacuum filter 17 reaches
During setting value (1kPa~0.09MPa), voltage transformation controller 13 automatically switches to the first filter 15 and filtered, to the second vacuum
Filter 17 is eluted, overturn, being purged, being overturn again；First vacuum filter 15 is made and second true by voltage transformation controller 13
Air filter 17 mutually switches.
2nd, coal tar fraction separating technology flow
Referring to Fig. 2, the internal solvent extract of solvent extract storage tank 18 is added to the preheating of the first tubular type through the 4th valve 19
In device 20, it is preheated to after 40~100 DEG C and equably sprays solvent extract (i.e. coal tar mixed liquor) through the 3rd sprayer 21
In the first decompression vaporizer 22, the first decompression vaporizer 22 top solvent vapo(u)r enters in the first condensing unit 23, condensed
Flow into afterwards in solvent tank 2, de- dross coal tar enters in de- dross coal tar storage tank 24 obtained by the first decompression vaporizer 22 bottom, takes off
Dross coal tar is pumped into the second tubular preheater 27 after being forced into 0.2~10MPa through de- dross coal tar feed pump 25, is preheated to
De- dross coal tar is equably sprayed in the second decompression vaporizer 29 through the 4th sprayer 28 after 100~600 DEG C, second subtracts
The pressure top light component of vaporizer 29 enters in coal tar light components storage tank 32 after being condensed into the second condensing unit 31,
Coal tar heavy component obtained by second decompression vaporizer 29 bottom enters in coal tar heavy component storage tank 30.
Heretofore described solvent is tetrahydrofuran, dichloromethane or toluene.
The present invention can realize that coal tar takes off the continuous operation of slag technique and the continuous separation of cut, obtain coal tar heavy group
Divide and coal tar light components are product.
First filter 15 and the top of the second filter 17 are passed through nitrogen, and the filter residue on filter screen is purged.
The first vacuum filter 15 is set mutually to switch with the second vacuum filter 17 by transformation automatic controller 13.
First rotary sprayer 14, the second rotary sprayer 16, the 3rd rotary sprayer 21 and the 4th rotary sprayer
28 can be such that coal oil mixture uniformly sprays.
The temperature range of first tubular preheater 20 preheating solvent extract is 40~100 DEG C.
First decompression vaporizer 22 internal upper part setting column plate, its number of plates is 5~8 pieces, pressure limit 1kPa~
0.09MPa。
The temperature range of the de- dross coal tar of second tubular preheater 27 preheating is 100~600 DEG C.
Second decompression vaporizer 29 internal upper part setting column plate, its number of plates is 8~12 pieces, pressure limit 1kPa~
0.09MPa。
The moulding pressure scope of solvent feed pump 4 is 0.2~0.5MPa.
The moulding pressure scope of solvent extract feed pump 11 is 0.2MPa~0.5MPa.
The de- moulding pressure scope of dross coal tar feed pump 25 is 0.2MPa~10MPa.
First vacuum filter 15 and the pressure limit 1kPa of the second vacuum filter 17~0.09MPa.
Filter screen is acidproof corrosion resistant braid fabric or ceramic filter screen, and aperture is 25~75um；
First rotary sprayer 14, the second rotary sprayer 16, the 3rd rotary sprayer 21 and the 4th rotary sprayer
28 gun slot is 75~100um；The rotating speed of first rotary sprayer 14 and second turn of rotary sprayer 16 is 10~100r/
min；The rotating speed of 3rd rotary sprayer 21 and the 4th turn of rotary sprayer 28 is 10~50r/min.
Condensing agent used in first condensing unit 23 and the second condensing unit 31 is water, methanol, liquefied ammonia or ethanol.
In order to illustrate the effect of the present invention, example 1 below takes off coalite tar during slag technique is carried out using coal tar and taken off
Slag is tested, and calculates de- slag rate (relative to dehydrated coal tar amount).Low temperature during embodiment 2 is carried out using coal tar fraction separating technology
Coal tar fraction separation test, in order to accurate Analyze ＆ separate product, using gas chromatograph-mass spectrometer (GC-MS) and thermal analyzer
Composition and thermal weight loss process to product are measured.The existing coal tar using experimental raw to be derived from semi-coke factory of northern Shensi Shenmu County
(heavy oil) is separated as experimental subjects, and the fundamental property that heavy oil (tar depositing reservoir subsurface layer oil) is determined by national standard is shown in Table 1.
The fundamental property of the coal tar heavy oil of table 1
Note：* minusing
Slag and cut continuous separation technology are taken off using coal tar of the present invention, selection tetrahydrofuran solvent is extractant, to coal
Tar be fractionated obtaining coal tar heavy component, coal tar light components.
Embodiment 1
It is 1 by volume to take 200g dehydrated coal tars：1 adds tetrahydrofuran solvent, after being stirred with glass bar, through taking out
Filter, centrifugation removing tar slag, a small amount of solvent in tar slag in filter paper and centrifuge tube are volatilized clean, calculated after weighing de-
Slag rate (relative to dehydrated coal tar amount) is 0.12%.The 200g dehydrated coal tars are taken to be by volume with tetrahydrofuran solvent again
1：1 is added in the coal tar extractive reaction kettle of the device, is tested according to foregoing schemes, weighs in tar slag storage tank and stores up
It is 0.3% that the tar slag deposited, which calculates de- slag rate (relative to dehydrated coal tar amount),.
In summary, it is known that take off slag and the de- slag contrast in laboratory using the device, the device coal tar takes off slag more thoroughly, and
It will not be caused damage because solvent volatilizees.
Embodiment 2
A certain amount of dehydrated coal tar is taken to be tested according to foregoing schemes, the temperature of the second tubular preheater is set respectively
For 200 DEG C, 300 DEG C, after off-test and respectively light by 1 to the middle coalite tar obtained from products pot (>=200 DEG C evaporate
Point), weigh 1 (≤200 DEG C of cuts), light by 2 (>=300 DEG C of cuts), 2 (≤300 DEG C of cuts) each 1mL are weighed, then with the two of 2mL
Chloromethanes dissolves, and then carries out GC-MS and TG analyses, and analysis result is shown in Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Figure 10
And table 2, table 3, table 4 and table 5.
Take a certain amount of dehydrated coal tar to enter the device, de- dross coal tar is obtained after de- slag, desolventizing and enters the second pipe
Formula preheater is preheated to 200 DEG C, carries out cutting cut under the second decompression vaporizer decompression state, obtains middle coalite tar light by 1
(≤200 DEG C of cuts) and weight 1 (>=200 DEG C of cuts), is detected by GC-MS and TG, analysis result such as Fig. 3, Fig. 4, Fig. 5,
Shown in Fig. 6 and table 2, table 3.It can be obtained by Fig. 3, Fig. 4 and the combination of table 2, middle coalite tar light 1 is that weight-loss ratio reaches at 200 DEG C
98.27%, illustrate that light 1 is almost detected completely by GC-MS, product is concentrated mainly on before 40min (retention time)；
It can be obtained by Fig. 5, Fig. 6 and the combination of table 3, middle coalite tar weighs 1 and reaches 4.17% in 200 DEG C of weight-loss ratios, is reached in 300 DEG C of weight-loss ratios
To 74.94%, illustrate that weight 1 only has part to be detected by GC-MS, product is concentrated mainly on after 40min (retention time).
Take a certain amount of dehydrated coal tar to enter the device, de- dross coal tar is obtained after de- slag, desolventizing and enters the second pipe
Formula preheater is preheated to 300 DEG C, carries out cutting cut under the second decompression vaporizer decompression state, obtains middle coalite tar light by 2
(≤300 DEG C of cuts) and weight 2 (>=300 DEG C of cuts), is detected by GC-MS and TG, analysis result such as Fig. 7, Fig. 8, Fig. 9,
Shown in Figure 10 and table 4, table 5.It can be obtained by Fig. 7, Fig. 8 and the combination of table 4, middle light 2 weight-loss ratio of coalite tar reaches 94.37%, says
Bright light 2 are almost detected completely by GC-MS, and retention time has product before 80min；By Fig. 9, Figure 10 and the knot of table 5
Conjunction can be obtained, and middle coalite tar weighs 2 weight-loss ratios and reaches 4.02%, illustrates that weight 2 can hardly be detected by GC-MS, be retained
Time product before 80min is seldom.
In summary, it is known that coal tar is fractionated using the device, fractionating effect is preferable.
Light 1 composition of coalite tar in table 2
Coalite tar weighs 1 and constituted in table 3
Light 2 composition of coalite tar in table 4
Coalite tar weighs 2 and constituted in table 5
From Fig. 4, Fig. 5 and Fig. 6 experimental studies results, slag and fraction seperation technique are taken off using the coal tar of the present invention
With device, the heavy component obtained in coal tar, light components can be efficiently separated, compared with conventional method, the present invention is one
The method for planting the continuous separation coal tar of green, the relatively conventional separator of device takes up an area small, small investment, is easily achieved industrialization.
Simultaneously instant invention overcomes energy consumption present in existing coal tar processing process is big, trivial operations, low separation efficiency, pollution environment
The problems such as.
Claims (10)
1. a kind of coal tar takes off slag and fraction seperation device, it is characterised in that extract including dehydrated coal tar storage tank (1), coal tar
Take reactor (6), solvent tank (2), solvent extract storage tank (18), the first tubular preheater (20), the first decompression vaporizer
(22), the second tubular preheater (27) and the second decompression vaporizer (29)；
Dehydrated coal tar storage tank (1) is connected with coal tar extractive reaction kettle (6) top entry, coal tar extractive reaction kettle (6)
Outlet at bottom is connected with solid-liquid separator (7) top entry, solid-liquid separator (7) outlet at bottom and solvent extract feed pump
(11) entrance is connected, and solvent extract feed pump (11) outlet is connected through voltage transformation controller (13) with two filters, each
Filter is connected with tar slag storage tank (10) and solvent extract storage tank (18)；
Solvent tank (2) outlet is divided into two-way, be connected all the way with coal tar extractive reaction kettle (6) top entry, another road with
Voltage transformation controller (13) is connected；
Solvent extract storage tank (18) outlet is connected with the first tubular preheater (20) entrance, the first tubular preheater (20) outlet
It is connected with first decompression vaporizer (22) entrance, the first decompression vaporizer (22) outlet at bottom and the second tubular preheater (27)
Entrance is connected, and the second tubular preheater (27) outlet is connected with second decompression vaporizer (29) entrance, the second decompression vaporizer
(29) top exit is connected with the second condensing unit (31).
2. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, it is characterised in that two filter bags
Include the first filter (15), the second filter (17), voltage transformation controller (13) and the first filter (15), the second filter (17)
Top entry is connected, and the outlet at bottom of the first filter (15) is divided into two-way, is connected all the way with tar slag storage tank (10), separately
It is connected all the way with solvent extract storage tank (18)；Second filter (17) outlet at bottom is divided into two-way, is stored up all the way with tar slag
Tank (10) is connected, and another road is connected with solvent extract storage tank (18).
3. a kind of coal tar according to claim 2 takes off slag and fraction seperation device, it is characterised in that the first filter
(15) porch is provided with the first rotary sprayer (14), and the second filter (17) porch is provided with the second rotary sprayer
(16), first decompression vaporizer (22) porch is provided with the 3rd rotary sprayer (21), second decompression vaporizer (29) entrance
Place is provided with the 4th rotary sprayer (28).
4. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, it is characterised in that solid-liquid separator
(7) outlet at bottom is also connected with vacuum flasher (8) top entry, on vacuum flasher (8) the condensed device of side outlet (9) with
Solvent extract feed pump (11) entrance is connected, and vacuum flasher (8) outlet at bottom is connected with tar slag storage tank (10).
5. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, it is characterised in that the first decompression vaporization
Room (22) top exit is connected with the first condensing unit (23) entrance, the first condensing unit (23) outlet at bottom and solvent tank
(2) it is connected.
6. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, it is characterised in that the first decompression vaporization
Room (22) outlet at bottom is connected through de- dross coal tar storage tank (24) with the second tubular preheater (27) entrance；Dehydrated coal tar storage tank
(1), solvent tank (2), tar slag storage tank (10), solvent extract storage tank (18), de- dross coal tar storage tank (24), coal tar heavy duty
Liquid level gauge is provided with inside matter component storage tank (30) and coal tar light components storage tank (32).
7. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, it is characterised in that the second condensing unit
(31) outlet at bottom is connected with coal tar light components storage tank (32) entrance；Second decompression vaporizer (29) outlet at bottom and coal
Tar heavy component storage tank (30) entrance is connected.
8. a kind of coal tar takes off slag and fraction seperation technique, it is characterised in that comprise the following steps：
1) coal tar takes off slag technological process
Injected after dehydrated coal tar is preheated in coal tar extractive reaction kettle (6), while solvent is heated and added by solvent tank (2)
It is pumped into after pressure in coal tar extractive reaction kettle (6)；In coal tar extractive reaction kettle (6) after heating, extraction, by solvent and dehydration
Coal oil mixture is separated through solid-liquid separator (7), obtains tar slag and solvent extract；
Solvent extract is added in the first filter (15) through the first rotating spraying (14) and filtered, and filtrate extracts into solvent
Take thing storage tank (18)；When the internal pressure of the first filter (15) reaches setting value, automatically switched by voltage transformation controller (13)
Filtered to the second filter (17), be passed through solvent and the filter screen in the first filter (15) is cleaned, when the second vacuum
When filter (17) internal pressure reaches setting value, the first filter (15) is automatically switched to by voltage transformation controller (13) and carried out
Filter, and be passed through solvent and the second vacuum filter (17) is cleaned；First vacuum filter is made by voltage transformation controller (13)
(15) mutually switch with the second vacuum filter (17)；
2) coal tar fraction separating technology flow
Solvent extract storage tank (18) internal solvent extract is added in the first tubular preheater (20), is sprayed at after preheating
In one decompression vaporizer (22), solvent vapo(u)r enters in the first condensing unit (23) at the top of the first decompression vaporizer (22), through cold
Flowed into after solidifying in solvent tank (2), the second tubular type is pumped into after de- dross coal tar pressurization obtained by first decompression vaporizer (22) bottom
In preheater (27), it is sprayed at after preheating in the second decompression vaporizer (29), light component is entered at the top of the second decompression vaporizer (29)
Enter and enter after the second condensing unit (31) is condensed in coal tar light components storage tank (32), second decompression vaporizer (29) bottom
Coal tar heavy component enters in coal tar heavy component storage tank (30) obtained by portion.
9. a kind of coal tar according to claim 8 takes off slag and fraction seperation technique, it is characterised in that solvent is tetrahydrochysene furan
Mutter, dichloromethane or toluene；The temperature of first tubular preheater (20) preheating solvent extract is 40~100 DEG C；Described first
Depressurize vaporizer (22) internal upper part and column plate is set, the number of plates is 5~8 pieces, pressure limit 1kPa~0.09MPa；Second tubular type is pre-
The temperature of the hot de- dross coal tar of device (27) preheating is 100~600 DEG C；Second decompression vaporizer (29) internal upper part sets column plate, tower
Plate number is 8~12 pieces, pressure limit 1kPa~0.09MPa；Coal tar extractive reaction kettle (6) interior dehydrated coal tar and solvent volume
Than for 1：(0.5~2).
10. a kind of coal tar according to claim 8 takes off slag and fraction seperation technique, it is characterised in that the filter screen is
Acidproof corrosion resistant braid fabric or ceramic filter screen, aperture are 25~75um；First rotary sprayer (14), the second rotation spray
The gun slot of day with fog (16), the 3rd rotary sprayer (21) and the 4th rotary sprayer (28) is 75~100um；First rotation
Sprayer (14) and the rotating speed of second turn of rotary sprayer (16) are 10~100r/min；3rd rotary sprayer (21) and the 4th
The rotating speed for turning rotary sprayer (28) is 10~50r/min.
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