CN106978203B - 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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- CN106978203B CN106978203B CN201710237562.1A CN201710237562A CN106978203B CN 106978203 B CN106978203 B CN 106978203B CN 201710237562 A CN201710237562 A CN 201710237562A CN 106978203 B CN106978203 B CN 106978203B
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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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Abstract
A kind of coal tar takes off slag and fraction seperation technique and device, it mixed, extracted with coal tar using solvent in coal tar extraction 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 vaporizing chamber and condenses to obtain solvent and de- dross coal tar through the first condensing unit, and solvent is Ke Xunhuanliyong；De- dross coal tar enters the second decompression vaporizing chamber and condenses to obtain coal tar heavy component and coal tar light components through the second condensing unit.Take off slag and fraction seperation technique and device the object of the present invention is to provide a kind of coal tar, the technique can realize coal tar oil ingredient it is effective be fractionated, process energy consumption is low, non-wastewater discharge, equipment investment are 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 technique
With rapid economic development, China has become world energy sources consumption big country, and demand of the market to oil product is increasingly
Increase, oil supply deficiency is outstanding day by day, and it is imperative to seek new alternative energy source.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,
Almost all of carbazole and quinoline all derive from coal tar in the market, and most of anthracene, acenaphthene and pyrene are also to pass through from coal tar
Processing, separation, extraction obtain.It can be seen that 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 that coking easily occurs, blocking pipeline, has a degree of influence on process equipment and catalyst etc., so being pre-processed in coal tar
It is vital that slag is taken off in stage.Coal tar takes off slag technology and has at present: solvent extraction and separation, emchanically centrifugal separation, pyrolysis point
From etc..When using emchanically centrifugal separation technology, since the coal-tar residue constituent difference of separate sources is larger, to adapt to centrifugation
The performance of machine is generally required and is further processed after coal-tar residue is pre-processed or is centrifuged, and is had and was operated
The disadvantages of journey is cumbersome, and cost of equipment is high.Coal Tars separation method is adaptable to coal-tar residue ingredient, hardly
Secondary pollution is caused, but it is higher to consume energy.
Important by-products of the coal tar as Coal dressing, be separated by distillation available light oil distillate, carbolic oil fraction,
Fraction of naphthalene oil, wash oil fraction, carbolineum fraction and pitch carry out being chemically treated available neutral component for first five kind fraction
(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, pesticide, fine chemistry industry and heat-resisting material.
Described in Chinese patent CN103102933A a kind of coal tar electro-desalting, dehydration, de- slag method, this method from
Sodium carbonate liquor is added in coal tar to be processed, is sufficiently mixed and the heating that exchanges heat, by coal tar after stable sodium salt to be formed
The filtering for carrying out mechanical admixture twice, filtered coal tar is continued to heat up, and water filling and demulsifier are carried out on pipeline, warp
After static mixer mixing, electro-desalting, dehydration equipment are finally entered, desalination is carried out under the action of high voltage electric field, dehydration, is taken off
Slag.The complex operation takes off slag low efficiency, 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, is suitble to
The pretreatment of low temperature or high temperature coal-tar, but the process low separation efficiency, complicated for operation, energy consumption is high.
A kind of dry distillation of coal and coal tar distillation combined technical method, feed coal are described in Chinese patent CN105647554A
Powder enters microwave treatment with the coal tar heavy end that Distallation systm is isolated after liquid is consolidated in mixing apparatus and is sufficiently mixed and reacts
Device generates coal gas, semicoke and coal tar；Coal tar enters Distallation systm after pretreatment and is separated into coal tar light fraction, coal tar
Oily heavy end and coal tar asphalt, coal tar heavy end, which is recycled back to liquid, to be consolidated mixing apparatus and mixes with coal dust.Coal in this method
Tar distillation cuts fraction low efficiency, and separation is not thorough, and the relatively narrow fraction of temperature range is not easy to cut.
A kind of efficient fractionating device, including fractionation room, heating device, temperature are described in Chinese patent CN205516583U
Sensing device, 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 operating condition of equipment in time, structure is excessively complicated, cumbersome, is unfavorable for extensive
Production.
In conclusion not only energy consumption is high for the de- slag of traditional coal tar and fraction seperation technique, various waste water are generated, to environment
A degree of pollution being caused, and separative efficiency is lower, separation is not thorough, and it is complicated for operation, it is time-consuming.So find it is pollution-free,
Low energy consumption, a kind of efficient coal tar take off slag and fraction seperation technology tool has very important significance.
Summary of the invention
In order to solve the problems, such as currently available technology, slag is taken off the object of the present invention is to provide a kind of coal tar and is evaporated
Point separating technology and device, the technique can realize coal tar oil ingredient it is effective be fractionated, process energy consumption is low, non-wastewater discharge, operation
Simply it is easily enlarged production scale.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of coal tar takes off slag and fraction seperation device, including dehydrated coal tar storage tank, coal tar extract reaction kettle, solvent
Storage tank, solvent extract storage tank, the first tubular preheater, the first decompression vaporizing chamber, the second tubular preheater and the second decompression
Vaporizing chamber；
Dehydrated coal tar storage tank is connected with coal tar extraction reaction kettle top entry, and coal tar extraction reactor bottom 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 extraction reaction kettle top entry, another way and change
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 vaporizing chamber top exit is connected with the second condensing unit.
A further improvement of the present invention lies in that two filters include first filter, the second filter, voltage transformation controller
Be connected with first filter, the second filter top entrance, the outlet at bottom of first filter is divided into two-way, all the way with tar
Slag storage tank is connected, and another way is connected with solvent extract storage tank；Second filter bottom outlet is divided into two-way, all the way with coke
Dregs of fat storage tank is connected, and another way is connected with solvent extract storage tank.
A further improvement of the present invention lies in that first filter inlet is provided with the first rotary sprayer, the second filtering
Device inlet is provided with the second rotary sprayer, is provided with the decompression of third rotary sprayer second at the first decompression chamber input
The 4th rotary sprayer is provided at chamber input.
A further improvement of the present invention lies in that solid-liquid separator outlet at bottom is also connected with vacuum flasher top entry
Logical, side outlet is connected through condenser with solvent extract charging pump intake on vacuum flasher, vacuum flasher outlet at bottom
It is connected with tar slag storage tank.
A further improvement of the present invention lies in that the first decompression vaporizing chamber top exit is connected with the first condensing unit entrance
Logical, the first condensing unit outlet at bottom is connected with solvent tank.
A further improvement of the present invention lies in 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 liquidometer.
A further improvement of the present invention lies in that 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, comprising the following steps:
1) coal tar takes off slag process flow
It is injected after dehydrated coal tar is preheated in coal tar extraction reaction kettle, while solvent is heated and pressurizeed by solvent tank
After be pumped into coal tar extraction reaction kettle in；In coal tar extraction reaction kettle after heating, extraction, solvent and dehydrated coal tar are mixed
It closes object to separate through solid-liquid separator, obtains tar slag and solvent extract；
Solvent extract is added in first filter through the first rotating spraying and is filtered, and filtrate enters solvent extract
Storage tank；When pressure inside first filter reaches setting value, the second filter is automatically switched to by voltage transformation controller and is carried out
Filtering, is passed through solvent and cleans to the strainer in first filter, when the second vacuum filter internal pressure reaches setting value
When, first filter is automatically switched to by voltage transformation controller and is filtered, and is passed through solvent and the second vacuum filter is carried out clearly
It washes；Switch the first vacuum filter mutually with the second vacuum filter by voltage transformation controller；
2) coal tar fraction separating technology process
Solvent extract storage tank internal solvent extract is added in the first tubular preheater, first is sprayed at after preheating and is subtracted
It presses in vaporizing chamber, solvent vapo(u)r enters in the first condensing unit at the top of the first decompression vaporizing chamber, and solvent tank is flowed into after condensing
In, it is pumped into the second tubular preheater after taking off the pressurization of dross coal tar obtained by the first decompression bottom of vaporizing chamber, the is sprayed at after preheating
In two decompression vaporizing chambers, light component enters light into coal tar after the second condensing unit is condensed at the top of the second decompression vaporizing chamber
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.
A further improvement of the present invention lies in that solvent is tetrahydrofuran, methylene chloride or toluene；First tubular preheater is pre-
The temperature of hot solvent extract is 40~100 DEG C；Column plate is arranged in the first decompression vaporizing chamber internal upper part, and the number of plates is 5~8
Block, pressure limit 1kPa~0.09MPa；The temperature that second tubular preheater preheats de- dross coal tar is 100~600 DEG C；Second
It depressurizes vaporizing chamber internal upper part and column plate is set, the number of plates is 8~12 pieces, pressure limit 1kPa~0.09MPa；Coal tar extraction reaction
Dehydrated coal tar and solvent volume ratio are 1:(0.5~2 in kettle).
A further improvement of the present invention lies in that the strainer is acidproof corrosion resistant braid fabric or ceramic filter screen, hole
Diameter is 25~75um；First rotary sprayer, the second rotary sprayer, third rotary sprayer and the 4th rotary sprayer
Gun slot be 75~100um；The revolving speed of first rotary sprayer and second turn of rotary sprayer is 10~100r/min；The
The revolving speed of three rotary sprayers and the 4th turn of rotary sprayer is 10~50r/min.
Compared with prior art, it the invention has the benefit that the present invention extracts reaction kettle by setting coal tar, adopts
It is extracted in coal tar extraction reaction kettle with solvent and dehydrated coal tar, is separated by solid-liquid separator, then existed
Two filters further remove the gred, and carry out through the first decompression vaporizing chamber except solvent, then carry out coal tar through the second decompression vaporizing chamber
Component fractionation obtains coal tar heavy component and coal tar light components.The present apparatus takes up little area, and structure is simple, at low cost, is easy to
Realize industrialization, solvent can be recycled, not generate waste water and pollute the environment, and can be realized coal tar and take off slag and evaporate
Divide separating technology continuous operation.
Further, by the way that vacuum flasher is arranged, solvent extract in tar slag can be made further to be separated.
Further, by setting first filter and the second filter, the first mistake is enabled to using voltage transformation controller
Filter and the second filter mutually switch automatically, and de- slag technique is made to realize continuous operation.
Further, pass through the first rotary sprayer of setting, the second rotary sprayer, third rotary sprayer, the 4th rotation
Turning sprayer disperses coal tar and its mixture well.
Dehydrated coal tar, solvent are added in coal tar extraction reaction kettle by the present invention, in coal tar extraction reaction kettle
After heating, extraction, solvent is separated with dehydrated coal tar mixture through solid-liquid separator, tar slag and solvent extraction are tentatively obtained
Object；Tar slag addition vacuum flasher is further obtained into tar slag component and solvent extract, by solvent extract through first
Tar slag component and solvent extract is further obtained by filtration in filter, the second filter；Gained solvent extract is added to
After the preheating of first tubular preheater, entering the vaporization of the first decompression vaporizing chamber separates solvent with coal tar, solvent vapo(u)r
It is condensed into the first condensing unit, obtains solvent, obtain de- dross coal tar in the first decompression bottom of vaporizing chamber；By de- dross coal tar
After being added to the preheating of the second tubular preheater, entering the vaporization of the second decompression vaporizing chamber separates coal tar oil ingredient, lightweight
Component is condensed into the second condensing unit, obtains coal tar light components, obtains coal tar heavy duty in the second decompression bottom of vaporizing chamber
Matter component；The present invention can be realized the continuous separation that coal tar takes off slag technique continuous operation and fraction, obtain coal tar heavy group
Divide and coal tar light components.With effective fractionation, process energy consumption is low, non-wastewater discharge, equipment investment is few, continuous production is easy
In expand the scale of production the advantages of, overcome coal tar in the prior art take off it is existing during slag and fraction seperation energy consumption is high,
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 mild, easy, and technique and equipment manufacturing cost are low.
Further, the first rotary sprayer, the second rotary sprayer, third rotary sprayer and the 4th rotating spraying
Device can be such that coal oil mixture uniformly sprays.
Detailed description of the invention
Fig. 1 is that coal tar of the invention takes off slag process flow；
Fig. 2 is coal tar fraction separating technology process of the invention；
Fig. 3 is the total ion chromatogram of light 1 component of middle coalite tar；
Fig. 4 is that the TG of light 1 component of middle coalite tar schemes；
Fig. 5 is the total ion chromatogram that middle coalite tar weighs 1 component；
Fig. 6 is the TG figure that middle coalite tar weighs 1 component；
Fig. 7 is the total ion chromatogram of light 2 component of middle coalite tar；
Fig. 8 is that the TG of light 2 component of middle coalite tar schemes；
Fig. 9 is the total ion chromatogram that middle coalite tar weighs 2 components；
Figure 10 is the TG figure that middle coalite tar weighs 2 components；
In figure, 1, dehydrated coal tar storage tank；2, solvent tank；3, the first valve；4, solvent feed pumps；5, the second valve；
6, coal tar extracts reaction kettle；7, solid-liquid separator；8, vacuum flasher；9, condenser；10, tar slag storage tank；11, solvent extracts
Take object feed pump；12, third valve；13, voltage transformation controller；14, the first rotary sprayer；15, first filter；16, second
Rotary sprayer；17, the second filter；18, solvent extract storage tank；19, the 4th valve；20, the first tubular preheater；21,
Third rotary sprayer；22, the first decompression vaporizing chamber；23, the first condensing unit；24, dross coal tar storage tank is taken off；25, dross coal is taken off
Tar feed pump；26, the 5th valve；27, the second tubular preheater；28, the 4th rotary sprayer；29, the second decompression vaporizing chamber；
30, coal tar heavy component storage tank；31, the second condensing unit；32, coal tar light components storage tank.
Specific embodiment
Below in conjunction with attached drawing, by embodiment, present invention is further described in detail.
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
Liquidometer 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 extraction reaction kettle 6, vacuum flasher 8, first filter 15, second filter
Device 17, the first tubular preheater 20, the second tubular preheater 27, first decompression vaporizing chamber 22, second depressurize the equal band of vaporizing chamber 29
There is heating mantle, the specific preheating temperature of solvent, can be set according to specific solvent in the present invention.
Dehydrated coal tar storage tank 1, coal tar extract reaction kettle 6, solid-liquid separator 7, vacuum flasher 8；Solvent extract
Storage tank 18, the first tubular preheater 20, first depressurize vaporizing chamber 22, the first condensing unit 23；De- dross coal tar 24, the second tubular type
Preheater 27, second depressurizes vaporizing chamber 29, the second condensing unit 31 is cascaded structure；The first filter 15 and the second filtering
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 takes off slag and fraction seperation device includes: dehydrated coal tar storage tank 1, solvent storage
Tank 2, the first valve 3, solvent feed pump the 4, second valve 5, coal tar extracts reaction kettle 6, solid-liquid separator 7, vacuum flasher
8, condenser 9, tar slag storage tank 10, solvent extract feed pump 11, third valve 12, voltage transformation controller 13, the first rotation spray
Day with fog 14, first filter 15, the second rotary sprayer 16, the second filter 17, solvent extract storage tank 18, the 4th valve
19, it is burnt to depressurize vaporizing chamber 22, the first condensing unit 23, de- dross coal for the first tubular preheater 20, third rotary sprayer 21, first
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 vaporizing chamber 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 coal tar extraction 6 top entry of reaction kettle,
Coal tar extraction 6 outlet at bottom of reaction kettle is connected with 7 top entry of solid-liquid separator, and 7 outlet at bottom of solid-liquid separator is divided into
Two-way is connected with 8 top entry of vacuum flasher all the way, and side outlet is through condenser 9 and solvent extract on vacuum flasher 8
11 entrance of feed pump is connected；8 outlet at bottom of vacuum flasher is connected with tar slag storage tank 10；Another way and solvent extract
11 entrance of feed pump is connected, and solvent extract feed pump 11 is exported through third valve 12, voltage transformation controller 13 and first filter
15,17 top entry of the second filter is connected, and the outlet at bottom of first filter 15 is divided into two-way, all the way with tar slag storage tank
10 are connected, and another way is connected with solvent extract storage tank 18；Likewise, 17 outlet at bottom of the second filter is divided into two-way,
It is connected all the way with tar slag storage tank 10, another way is connected with solvent extract storage tank 18.
Solvent tank 2 outlet with solvent feed pump 4 entrances is connected, solvent feed pump 4 export is divided into two-way, all the way with coal tar
Oil extraction 6 top entry of reaction kettle is connected, and another way is through the second valve 5, voltage transformation controller 13 and first filter 15, second
17 top entry of filter is connected.
Referring to fig. 2, the outlet of solvent extract storage tank 18 is connected through the 4th valve 19 with 20 entrance of the first tubular preheater, the
The outlet of one tubular preheater 20 is connected with the first decompression 22 entrance of vaporizing chamber, the first decompression 22 top exit of vaporizing chamber and first
23 entrance of condensing unit is connected, and 23 outlet at bottom of the first condensing unit is connected with solvent tank 2；First decompression 22 bottom of vaporizing chamber
Portion outlet is connected with de- 24 entrance of dross coal tar storage tank, takes off the outlet of dross coal tar storage tank 24 warp and takes off dross coal tar feed pump 25, the
Five valves 26 are connected with 27 entrance of the second tubular preheater, the outlet of the second tubular preheater 27 and the second decompression 29 entrance of vaporizing chamber
It is connected, the second decompression 29 top exit of vaporizing chamber is connected with the second condensing unit 31,31 outlet at bottom of the second condensing unit and coal
32 entrance of tar light components storage tank is connected；Second decompression 29 outlet at bottom of vaporizing chamber and coal tar heavy component storage tank 30
Entrance is connected.
The setting of first rotary sprayer 14 is arranged in 15 inlet of first filter, the second rotary sprayer 16 in the second mistake
17 inlet of filter, the setting of third rotary sprayer 21 depressurize 22 inlet of vaporizing chamber first, and the 4th rotary sprayer 28 is set
It sets and depressurizes 29 inlet of vaporizing chamber second.
Coal tar of the invention take off slag and fraction seperation technique the following steps are included:
One, coal tar takes off slag process flow
It is injected referring to Fig. 1, after dehydrated coal tar is preheating to 40 DEG C~100 DEG C in coal tar extraction reaction kettle, while molten
Agent (tetrahydrofuran, methylene chloride or toluene) is forced into after being heated to 40 DEG C~100 DEG C by solvent tank 2 through solvent feed pump 4
It is pumped into after 0.2~0.5MPa in coal tar extraction reaction kettle 6；Coal tar extracts dehydrated coal tar and solvent volume in reaction kettle 6
Than for 1:(0.5~2)；
In coal tar extraction 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 enters vacuum flasher 8 and further obtains tar slag and solvent
Extract.
Through the isolated solvent extract of the isolated solvent extract of solid-liquid separator 7 and vacuum flasher 8
It is homogeneously added into first filter 15 and is filtered through the first rotating spraying 14, filtrate enters solvent extract storage tank 18；
When pressure inside first filter 15 reaches setting value (1kPa~0.09MPa), voltage transformation controller 13 automatically switches to
Tow filtrator 17 is filtered, be passed through solvent (tetrahydrofuran, methylene chloride or toluene) to the strainer in first filter 15 into
Row elution, leacheate enter solvent extract storage tank 18, strainer are overturn, the filter residue being passed through on nitrogen purging strainer, filter
Slag is stored in tar slag storage tank 10, again overturns strainer after purging is clean；When 17 internal pressure of the second vacuum filter reaches
When setting value (1kPa~0.09MPa), voltage transformation controller 13 automatically switches to first filter 15 and is filtered, to the second vacuum
Filter 17 is eluted, is overturn, is purged, is overturn again；Keep the first vacuum filter 15 and second true by voltage transformation controller 13
Air filter 17 mutually switches.
Two, coal tar fraction separating technology process
Referring to fig. 2,18 internal solvent extract of solvent extract storage tank is added to the preheating of the first tubular type through the 4th valve 19
In device 20, solvent extract (i.e. coal tar mixed liquor) is equably sprayed through third sprayer 21 after being preheated to 40~100 DEG C
In the first decompression vaporizing chamber 22, the first decompression 22 top solvent vapo(u)r of vaporizing chamber enters in the first condensing unit 23, through condensing
It flows into solvent tank 2 afterwards, takes off dross coal tar obtained by the first decompression 22 bottom of vaporizing chamber and enter in de- dross coal tar storage tank 24, take off
Dross coal tar is pumped into the second tubular preheater 27 after de- dross coal tar feed pump 25 is forced into 0.2~10MPa, is preheated to
De- dross coal tar is equably sprayed in the second decompression vaporizing chamber 29 through the 4th sprayer 28 after 100~600 DEG C, second subtracts
Pressure 29 top light component of vaporizing chamber enters after the second condensing unit 31 is condensed and enters in coal tar light components storage tank 32,
Coal tar heavy component obtained by second decompression 29 bottom of vaporizing chamber enters in coal tar heavy component storage tank 30.
Heretofore described solvent is tetrahydrofuran, methylene chloride or toluene.
The present invention can be realized the continuous separation that coal tar takes off slag technique continuous operation and fraction, obtain coal tar heavy group
Divide and coal tar light components are product.
It is passed through nitrogen at the top of first filter device 15 and the second filter device 17, the filter residue on strainer is purged.
Switch the first vacuum filter 15 can mutually with the second vacuum filter 17 by transformation automatic controller 13.
First rotary sprayer 14, the second rotary sprayer 16, third rotary sprayer 21 and the 4th rotary sprayer
28 can be such that coal oil mixture uniformly sprays.
The temperature range that first tubular preheater 20 preheats solvent extract is 40~100 DEG C.
First decompression 22 internal upper part of vaporizing chamber sets column plate, and the number of plates is 5~8 pieces, and pressure limit 1kPa~
0.09MPa。
The temperature range that second tubular preheater 27 preheats de- dross coal tar is 100~600 DEG C.
Second decompression 29 internal upper part of vaporizing chamber sets column plate, and the number of plates is 8~12 pieces, and pressure limit 1kPa~
0.09MPa。
It is 0.2~0.5MPa that solvent feed, which pumps 4 moulding pressure ranges,.
11 moulding pressure range of solvent extract feed pump is 0.2MPa~0.5MPa.
De- 25 moulding pressure range of dross coal tar feed pump is 0.2MPa~10MPa.
17 pressure limit 1kPa~0.09MPa of first vacuum filter 15 and the second vacuum filter.
Strainer is acidproof corrosion resistant braid fabric or ceramic filter screen, and aperture is 25~75um；
First rotary sprayer 14, the second rotary sprayer 16, third rotary sprayer 21 and the 4th rotary sprayer
28 gun slot is 75~100um；The revolving speed of first rotary sprayer 14 and second turn of rotary sprayer 16 is 10~100r/
min；The revolving speed of third 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 ethyl alcohol.
In order to illustrate effect of the invention, following example 1 takes off coalite tar in the progress of slag technique using coal tar and takes off
Slag test, calculates de- slag rate (relative to dehydrated coal tar amount).Embodiment 2 is using low temperature in the progress of 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.It is now the coal tar for being derived from semi-coke factory, northern Shensi Shenmu County with experimental raw
(heavy oil) is separated as experimental subjects, and heavy oil (tar clarifying basin subsurface layer oil) is shown in Table 1 by the fundamental property that national standard measures.
The fundamental property of 1 coal tar heavy oil of table
Note: * minusing
Slag and fraction continuous separation technology are taken off using coal tar of the present invention, select tetrahydrofuran solvent for extractant, to coal
Tar is fractionated to obtain coal tar heavy component, coal tar light components.
Embodiment 1
Taking 200g dehydrated coal tar by volume is that tetrahydrofuran solvent is added in 1:1, after mixing evenly 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, are calculated after weighing de-
Slag rate (relative to dehydrated coal tar amount) is 0.12%.The 200g dehydrated coal tar is taken to be by volume with tetrahydrofuran solvent again
1:1 is added in the coal tar extraction reaction kettle of the device, is tested according to foregoing schemes, weighs and store up in tar slag storage tank
It is 0.3% that de- slag rate (relative to dehydrated coal tar amount), which is calculated, in the tar slag deposited.
In summary, it is known that slag is taken off using the device and laboratory takes off slag comparison, which takes off slag more thoroughly, and
It will not cause damages 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 respectively set
For 200 DEG C, 300 DEG C, after the test and respectively to from middle coalite tar obtained in products pot, light by 1 (>=200 DEG C evaporate
Point), weigh 1 (≤200 DEG C of fractions), light by 2 (>=300 DEG C of fractions), weigh 2 (≤300 DEG C of fractions) each 1mL, then with the two of 2mL
Chloromethanes dissolution, then carries out GC-MS and TG analysis, 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.
It takes a certain amount of dehydrated coal tar into 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 fraction under the second decompression vaporizing chamber decompression state, it is light by 1 to obtain middle coalite tar
(≤200 DEG C of fractions) and weight 1 (>=200 DEG C of fractions) 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.By Fig. 3, Fig. 4 and table 2 in conjunction with that can obtain, middle coalite tar light 1 is that weight-loss ratio reaches at 200 DEG C
98.27%, illustrate that light 1 is almost detected that product is concentrated mainly on before 40min (retention time) by GC-MS completely；
By Fig. 5, Fig. 6 and table 3 in conjunction with that can obtain, middle coalite tar weighs 1 and reaches 4.17% in 200 DEG C of weight-loss ratios, reaches in 300 DEG C of weight-loss ratios
To 74.94%, illustrate that weight 1 is only partially detected by GC-MS, product is concentrated mainly on after 40min (retention time).
It takes a certain amount of dehydrated coal tar into 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 fraction under the second decompression vaporizing chamber decompression state, it is light by 2 to obtain middle coalite tar
(≤300 DEG C of fractions) and weight 2 (>=300 DEG C of fractions) 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.By Fig. 7, Fig. 8 and table 4 in conjunction with that can obtain, middle light 2 weight-loss ratio of coalite tar reaches 94.37%, says
Bright light 2 are almost detected that retention time has product before 80min by GC-MS completely；By Fig. 9, Figure 10 and 5 knot of table
Conjunction can obtain, and middle coalite tar weighs 2 weight-loss ratios and reaches 4.02%, illustrate that weight 2 can hardly be detected by GC-MS, retain
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 composition in table 3
Light 2 composition of coalite tar in table 4
Coalite tar weighs 2 compositions in table 5
By the experimental studies results of Fig. 4, Fig. 5 and Fig. 6 as it can be seen that taking off slag and fraction seperation technique using coal tar of the invention
With device, it can efficiently separate to obtain heavy component, light components in coal tar, be compared with the traditional method, the present invention is one
The method of the continuous separation coal tar of kind green, device take up little area with respect to conventional separating apparatus, small investment, are easily industrialized.
Energy consumption is high, trivial operations, low separation efficiency, pollution environment the present invention overcomes existing during existing coal tar processing simultaneously
The problems such as.
Claims (9)
1. a kind of coal tar takes off slag and fraction seperation device, which is characterized in that extract including dehydrated coal tar storage tank (1), coal tar
Take reaction kettle (6), solvent tank (2), solvent extract storage tank (18), the first tubular preheater (20), the first decompression vaporizing chamber
(22), the second tubular preheater (27) and the second decompression vaporizing chamber (29)；
Dehydrated coal tar storage tank (1) is connected with coal tar extraction reaction kettle (6) top entry, and coal tar extracts 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, all the way with coal tar extraction reaction kettle (6) top entry be connected, another way 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 vaporizing chamber (22) entrance, the first decompression vaporizing chamber (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 vaporizing chamber (29) entrance, the second decompression vaporizing chamber
(29) top exit is connected with the second condensing unit (31)；
Two filters include first filter (15), the second filter (17), voltage transformation controller (13) and first filter
(15), the second filter (17) top entry is connected, and the outlet at bottom of first filter (15) is divided into two-way, all the way with tar
Slag storage tank (10) is connected, and another way is connected with solvent extract storage tank (18)；Second filter (17) outlet at bottom is divided into
Two-way is connected with tar slag storage tank (10) all the way, and another way is connected with solvent extract storage tank (18).
2. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, which is characterized in that first filter
(15) inlet is provided with the first rotary sprayer (14), and the second filter (17) inlet is provided with the second rotary sprayer
(16), first decompression vaporizing chamber (22) inlet is provided with third rotary sprayer (21), second decompression vaporizing chamber (29) entrance
Place is provided with the 4th rotary sprayer (28).
3. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, which is characterized in that solid-liquid separator
(7) outlet at bottom is also connected with vacuum flasher (8) top entry, on vacuum flasher (8) side outlet through condenser (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).
4. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, which is characterized 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.
5. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, which is characterized 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
Liquidometer is provided with inside matter component storage tank (30) and coal tar light components storage tank (32).
6. a kind of coal tar according to claim 1 takes off slag and fraction seperation device, which is characterized in that the second condensing unit
(31) outlet at bottom is connected with coal tar light components storage tank (32) entrance；Second decompression vaporizing chamber (29) outlet at bottom and coal
Tar heavy component storage tank (30) entrance is connected.
7. a kind of coal tar takes off slag and fraction seperation technique, which comprises the following steps:
1) coal tar takes off slag process flow
It is injected in coal tar extraction reaction kettle (6) after dehydrated coal tar is preheated, while solvent is heated and added by solvent tank (2)
It is pumped into after pressure in coal tar extraction reaction kettle (6)；In coal tar extraction 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 first filter (15) through the first rotating spraying (14) and is filtered, and filtrate enters solvent extraction
Take object storage tank (18)；When the internal pressure of first filter (15) reaches setting value, automatically switched by voltage transformation controller (13)
It is filtered to the second filter (17), is passed through solvent and the strainer in first filter (15) is cleaned, when the second filtering
When device (17) internal pressure reaches setting value, first filter (15) is automatically switched to by voltage transformation controller (13) and is filtered,
And it is passed through solvent and the second filter (17) is cleaned；Make first filter (15) and the second mistake by voltage transformation controller (13)
Filter (17) mutually switches；
2) coal tar fraction separating technology process
Solvent extract storage tank (18) internal solvent extract is added in the first tubular preheater (20), is sprayed at after preheating
In one decompression vaporizing chamber (22), solvent vapo(u)r enters in the first condensing unit (23) at the top of the first decompression vaporizing chamber (22), through cold
It is flowed into solvent tank (2) after solidifying, is pumped into the second tubular type after taking off the pressurization of dross coal tar obtained by first decompression vaporizing chamber (22) bottom
In preheater (27), be sprayed at after preheating in the second decompression vaporizing chamber (29), second decompression vaporizing chamber (29) at the top of light component into
Enter and enters in coal tar light components storage tank (32) after the second condensing unit (31) is condensed, second decompression vaporizing chamber (29) bottom
Coal tar heavy component obtained by portion enters in coal tar heavy component storage tank (30).
8. a kind of coal tar according to claim 7 takes off slag and fraction seperation technique, which is characterized in that solvent is tetrahydro furan
It mutters, methylene chloride or toluene；The temperature that first tubular preheater (20) preheats solvent extract is 40~100 DEG C；Described first
It depressurizes vaporizing chamber (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 that hot device (27) preheats de- dross coal tar is 100~600 DEG C；Column plate, tower is arranged in second decompression vaporizing chamber (29) internal upper part
Plate number is 8~12 pieces, pressure limit 1kPa~0.09MPa；Coal tar extracts reaction kettle (6) interior dehydrated coal tar and solvent volume
Than for 1:(0.5~2).
9. a kind of coal tar according to claim 7 takes off slag and fraction seperation technique, which is characterized in that the strainer is resistance to
The corrosion resistant braid fabric of acid or ceramic filter screen, aperture are 25~75um；First rotary sprayer (14), the second rotating spraying
The gun slot of device (16), third rotary sprayer (21) and the 4th rotary sprayer (28) is 75~100um；First rotation spray
Day with fog (14) and the revolving speed of second turn of rotary sprayer (16) are 10~100r/min；Third rotary sprayer (21) with the 4th turn
The revolving speed of rotary sprayer (28) is 10~50r/min.
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| CN105018124A (en) * | 2015-07-15 | 2015-11-04 | 太原市金浦顺化工有限公司 | Coal tar waste-residue extraction separation method |
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| CN103275754A (en) * | 2013-05-30 | 2013-09-04 | 神华集团有限责任公司 | Method for separating liquefied heavy oil and asphalt substrate from direct coal liquefaction residues |
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