CN206591082U - A kind of coal tar fraction separator - Google Patents
A kind of coal tar fraction separator Download PDFInfo
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- CN206591082U CN206591082U CN201720192847.3U CN201720192847U CN206591082U CN 206591082 U CN206591082 U CN 206591082U CN 201720192847 U CN201720192847 U CN 201720192847U CN 206591082 U CN206591082 U CN 206591082U
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Abstract
A kind of coal tar fraction separator, including the first paste state bed reactor and the first vacuum filter, first paste state bed reactor top at the top of the first vacuum filter with being connected, first vacuum filter motor spindle is divided into two-way, it is connected all the way with the remaining part storage tank of solvent orange 2 A extraction absorption, it is connected at the top of another paste state bed reactors of Lu Yu tri-, the 3rd paste state bed reactor top at the top of the 3rd vacuum filter with being connected, and the 3rd vacuum filter motor spindle is connected with solvent B elution fraction storage tanks；Solvent B elution fractions storage tank is connected with crude phenols knockout tower, and the remaining part storage tank of solvent orange 2 A extraction absorption is connected with neutral oil knockout tower.The utility model is green separation technique, and waste water, waste residue and waste gas are not produced, and solvent can be recycled, and the operating condition of technique is gentle, easy, technique and equipment manufacturing cost is low, less investment the advantages of.
Description
Technical field
The utility model belongs to technical field of coal chemical industry, is related to a kind of coal tar fraction separator.
Background technology
Coal tar is one of staple product of coking industry, and its yield accounts for the 3%~4% of shove charge coal, and it is constituted extremely
Complexity, be in most cases by coal-tar industry exclusively carry out separation, purification after be used.Coal tar is according to chemical composition master
To include neutral compound (mainly including aromatic hydrocarbon and aliphatic compound) and acid compound.Neutral compound is also known as
Neutral oil, compound fragrant hydrocarbon has the high added values such as naphthalene, anthracene, phenanthrene and the pyrene that petrochemical industry can not obtain or be not directly available
Fine chemicals；Aliphatic compound is the important component of the fuel oil such as gasoline, diesel oil, is that hydrogenation produces high hexadecane
It is worth the good raw material of diesel oil.Acid compound is primarily referred to as the phenolic compound in coal tar, and phenolic compound is important change
Work raw material and high value added product, can manufacture agricultural chemicals, medicine, resin, dyestuff etc..Therefore, isolated from coal tar content compared with
High neutral compound and acid compound is very necessary.
Coal tar isolation technics includes distillation and rectifying, crystallization, absorption, UF membrane and solvent extraction etc., wherein, distillation
All it is the method that each component is separated using boiling point difference with rectifying, but its energy consumption is big, and temperature is too high also to be caused in coal tar
Some decomposition of components；Crystallization technique is close for some boiling points, and crystalline temperature differs the separating effect of larger thing system substantially, but right
It is restricted in the separating capacity of this polynary complex component of coal tar；Adsorb and membrane separation technique is according to filler in knockout tower
The difference of absorption property, makes the component of certain in mobile phase be separated from mixed system, due to coal tar poor fluidity, causes this
Method low separation efficiency；Solvent extraction is a kind of different separation methods of utilization different material solubility in selected solvent,
But this method solvent load is larger, corrosion is easily caused to equipment.
Chinese patent CN105368473A methods describeds are a kind of coal tar fraction separator and separating technology, with silica gel
Extract and separate is carried out for the chromatographic column method of filler, elution point is carried out to the coal tar fraction for removing asphalt component using two kinds of solvents
From, then through distilling column distillation processing, respectively obtain neutral oil ingredient and crude phenols component.Silica gel can not in the utility model chromatographic column
It is mobile, make to remain coal tar fraction in silica gel, cause the reduction of coal tar fraction separative efficiency.
A kind of separator of coal tar is described in Chinese patent CN204958816U, the separator leads to from top to down
Cross heating tube heat supply to separate the cut of different flash-points, each cut upper end is communicated with accumulator tank and temperature reducing unit, but should
Device can not be fully by the fraction seperation of different flash-points, and is difficult control temperature, is unfavorable for being sufficiently separated for coal tar.
Chinese patent CN105419837A describes a kind of coal carbonaceous residues extraction separating method, and the utility model passes through super
Sound wave auxiliary extraction, melt cinder are separated, organic matter is enriched with and the recycling step of extractant carries out extract and separate to coal carbonaceous residues,
Reacted under normal temperature and pressure using carbon dioxide, water, extractant and realize organic matter is extracted in coal carbonaceous residues, destroyed after heating
The system of the generation, so that separation is realized, but ultrasonic extraction efficiency is low, finally generates waste water, pollutes environment.
Chinese patent CN103111088A describes in a kind of extraction separation and Extraction the complete of phenols in coalite tar
Equipment, the equipment is made up of five kettles, four tanks and three groups of condensers, and refining crude is obtained using solvent extraction extract and separate
Phenol, but the equipment is complicated, to realize that industrialization also needs to further improvement.
In summary, not only energy consumption is big during traditional coal tar processing, low separation efficiency, and can produce substantial amounts of
Phenol wastewater, the problems such as causing environmental pollution.So, find low energy consumption, no pollution, a kind of efficient skill for separating coal tar
Art tool has very important significance.
Utility model content
The problem of to overcome in currently available technology, the purpose of this utility model is to provide a kind of coal tar fraction separation dress
Put, the separating technology can realize the low energy consumption of coal tar fraction, no pollution, high efficiency, be easily achieved industrialization.
To achieve these goals, the technical solution adopted in the utility model is as follows：
A kind of coal tar fraction separator, including the first paste state bed reactor and the first vacuum filter, the first slurry
Bed reactor top at the top of the first vacuum filter with being connected, and the first vacuum filter motor spindle is divided into two-way, extracts all the way with solvent orange 2 A
Take the remaining part storage tank of absorption to be connected, another road with being connected at the top of the second paste state bed reactor, the second paste state bed reactor bottom and
3rd paste state bed reactor is connected；3rd paste state bed reactor top at the top of the 3rd vacuum filter with being connected, the 3rd vacuum mistake
Filter bottom is divided into two-way, is connected all the way with solvent B elution fraction storage tanks, is connected at the top of another paste state bed reactors of Lu Yu tetra-；
Solvent B elution fractions storage tank is connected with crude phenols knockout tower, and the remaining part storage tank of solvent orange 2 A extraction absorption is connected with neutral oil knockout tower.
The utility model, which is further improved, to be, another paste state bed reactor of road second of the first vacuum filter motor spindle
It is connected with the second vacuum filter, the second vacuum filter motor spindle is divided into two-way, all the way with the remaining part storage tank of solvent orange 2 A extraction absorption
It is connected, is connected at the top of another paste state bed reactors of Lu Yu tri-.
The utility model further improve is, the 3rd vacuum filter motor spindle also with the 4th paste state bed reactor at the top of
It is connected, the 4th paste state bed reactor top is connected with the 4th vacuum filter；4th vacuum filter motor spindle is divided into two-way, all the way
It is connected with solvent B elution fraction storage tanks, another road at the top of the first paste state bed reactor with being connected.
The utility model, which is further improved, to be, crude phenols separate column overhead and phase at the top of crude phenols knockout tower overhead condenser
Even, crude phenols knockout tower overhead condenser bottom is connected with crude phenols knockout tower overhead reflux tank top, crude phenols knockout tower overhead reflux
Pot bottom is connected with crude phenols knockout tower overhead reflux pump intake, and crude phenols knockout tower overhead reflux pump discharge is divided into two-way, all the way with
Crude phenols separation column overhead is connected, and another road is connected with solvent B storage tanks.
The utility model, which is further improved, to be, crude phenols knockout tower bottom of towe is divided into two-way, all the way through crude phenols knockout tower tower
Bottom reboiler is connected with crude phenols knockout tower bottom of towe, and another road is connected with crude phenols component discharging condenser inlet, the discharging of crude phenols component
Condensator outlet is connected with crude phenols component discharging pump intake, and crude phenols component discharging pump discharge is connected with crude phenols storage tank.
The utility model, which is further improved, to be, neutral oil separation column and neutral oil knockout tower overhead condenser top
Portion is connected, and neutral oil knockout tower overhead condenser bottom is connected with neutral oil knockout tower overhead reflux tank top；Neutral oil is separated
Column overhead backflow pot bottom is connected with neutral oil knockout tower overhead reflux pump intake, neutral oil knockout tower overhead reflux pump discharge point
For two-way, it is connected all the way with neutral oil separation column, another road is connected with solvent orange 2 A storage tank.
The utility model, which is further improved, to be, neutral oil knockout tower bottom of towe is divided into two-way, is separated all the way through neutral oil
Tower tower bottom reboiler is connected with neutral oil knockout tower bottom of towe, and another road is connected with neutral oil ingredient discharging condenser inlet；It is neutral
Oil ingredient discharging condensator outlet is connected with neutral oil ingredient discharging pump entrance, and neutral oil ingredient discharging pump outlet is stored up with neutral oil
Tank is connected.
Compared with prior art, the utility model has the advantage that：The utility model is by setting the first slurry bed system
Reactor and the first vacuum filter, are extracted using solvent orange 2 A with coal tar fraction, silica gel in the first paste state bed reactor
Take, separated by the first vacuum filter, then rectifying is separated in neutral oil knockout tower, can obtain neutral oil group
Point；By setting the 3rd paste state bed reactor, the 3rd vacuum filter and crude phenols knockout tower, pass through the crude phenols of silica gel absorption
Solvent B is eluted, and is separated by the 3rd vacuum filter, and rectifying is separated in through crude phenols knockout tower, so as to obtain crude phenols group
Point.The present apparatus is simple in construction, and cost is low, can realize the separation of coal tar fraction.
Further, by setting the second paste state bed reactor, silica gel phenol can further be washed using solvent orange 2 A
Wash.
Further, by setting the 4th paste state bed reactor, eluting silica gel can be eluted using solvent B, obtained
To the silica gel that can be reused.
Further, by setting crude phenols knockout tower overhead condenser, crude phenols knockout tower return tank of top of the tower and crude phenols to separate
Column overhead reflux pump, can obtain reusable solvent B.
Further, by set neutral oil knockout tower overhead condenser, neutral oil knockout tower return tank of top of the tower and in
Property oil separation column overhead reflux pump, reusable solvent orange 2 A can be obtained.
Further, combined by the second paste state bed reactor with the second vacuum filter, pass through the second slurry reactor
Device and the second vacuum filter, which are combined, make it that the washing of silica gel phenol is abundant.
Brief description of the drawings
Fig. 1 is coal tar fraction of the present utility model separation solvent orange 2 A extraction absorbing process flow；
Fig. 2 is that coal tar fraction of the present utility model separates solvent B elution processes flows；
Fig. 3 is the remaining part of coal tar fraction of the present utility model separation absorption and elution fraction concentration technology flow；
Fig. 4 is the total ion chromatogram of neutral oil ingredient；
Fig. 5 is the total ion chromatogram of crude phenols component；
Fig. 6 is the influence that solvent orange 2 A elutes number of times centering oil residual phenol content；
Fig. 7 is that solvent B elutes influence of the number of times to phenol content in crude phenols；
In figure, 1, silica gel batcher；2nd, coal tar fraction storage tank；3rd, solvent orange 2 A storage tank；4th, the first valve；5th, the second valve；
6th, solvent orange 2 A feed pump；7th, the first paste state bed reactor；8th, the 3rd valve；9th, the 4th valve；10th, the first vacuum filter；11、
First silica gel phenol batcher；12nd, the second paste state bed reactor；13rd, the 5th valve；14th, the second vacuum filter；15th, the second silicon
Glue phenol batcher；16th, solvent B storage tanks；17th, the 6th valve；18th, solvent B feed pumps；19th, the 7th valve；20th, the 3rd slurry bed system
Reactor；21st, the 8th valve；22nd, the 3rd vacuum filter；23rd, the 3rd silica gel phenol batcher；24th, the 9th valve；25th, the 4th
Paste state bed reactor；26th, the 4th vacuum filter；27th, solvent B elution fractions storage tank；28th, solvent B elution fractions feed pump；29th, it is thick
Phenol knockout tower；30th, crude phenols knockout tower overhead condenser；31st, crude phenols knockout tower return tank of top of the tower；32nd, crude phenols separation column overhead is returned
Flow pump；33rd, crude phenols knockout tower tower bottom reboiler；34th, crude phenols component discharging condenser；35th, crude phenols component discharging pump；36th, crude phenols
Storage tank；37th, the remaining part storage tank of solvent orange 2 A extraction absorption；38th, the remaining part feed pump of solvent orange 2 A extraction absorption；39th, neutral oil knockout tower；
40th, neutral oil knockout tower overhead condenser；41st, neutral oil separation return tank of top of the tower；42nd, neutral oil knockout tower overhead reflux pump；
43rd, neutral oil knockout tower tower bottom reboiler；44th, neutral oil ingredient discharging condenser；45th, neutral oil ingredient discharging pump；46th, it is neutral
Oil tank.
Embodiment
The utility model is described in further detail by embodiment below in conjunction with accompanying drawing.
All raw materials, intermediate products and storage tank described in the utility model all carry Liquid level；The first described slurry
State bed reactor 7, the second paste state bed reactor 12, the 3rd paste state bed reactor 20, the 4th band heating of paste state bed reactor 25
Set；Described solvent orange 2 A storage tank 3 carries heating mantle with solvent B storage tanks 16；First paste state bed reactor 7, the second slurry bed system
Reactor 12, the 3rd paste state bed reactor 20, the 4th paste state bed reactor 25 and the first vacuum filter 10, the second vacuum filter
Machine 14, the 3rd vacuum filter 22, the 4th vacuum filter 26, silica gel batcher 1, the second silica gel phenol batcher 15 are tandem junctions
Structure.
Coal tar fraction is obtained by coalite tar, medium temperature coal tar or high temperature coal-tar depitching matter in the utility model
Coal tar；
Silica gel phenol of the present utility model is the abbreviation after aldehydes matter in silica gel absorption coal tar fraction.
Referring to Fig. 1, Fig. 2 and Fig. 3, a kind of coal tar fraction continuous separation device includes：Silica gel batcher 1, coal tar evaporate
Divide storage tank 2, solvent orange 2 A storage tank 3, solvent orange 2 A feed pump 6, the first paste state bed reactor 7, the first vacuum filter 10, the second slurry bed system
Reactor 12, the second vacuum filter 14, the second silica gel phenol batcher 15, solvent B storage tanks 16, solvent B feed pumps the 18, the 3rd are starched
State bed reactor 20, the 3rd vacuum filter 22, the 3rd silica gel phenol batcher 23, the 4th paste state bed reactor 25, the 4th vacuum
Filter 26, solvent B elution fractions storage tank 27, solvent B elution fractions feed pump 28, crude phenols knockout tower 29, crude phenols separation column overhead are cold
Condenser 30, crude phenols knockout tower return tank of top of the tower 31, crude phenols knockout tower overhead reflux pump 32, crude phenols knockout tower tower bottom reboiler 33,
It is crude phenols component discharging condenser 34, crude phenols component discharging pump 35, crude phenols storage tank 36, the remaining part storage tank 37 of solvent orange 2 A extraction absorption, molten
The remaining part charging 38 of agent A extraction absorption, neutral oil knockout tower 39, neutral oil knockout tower overhead condenser 40, neutral oil knockout tower
Top return tank 41, neutral oil knockout tower overhead reflux pump 42, neutral oil knockout tower tower bottom reboiler 43, neutral oil ingredient discharging are cold
Condenser 44, neutral oil ingredient discharging pump 45 and neutral oil tank 46.
Referring to Fig. 1, silica gel batcher 1 is connected through the first valve 4 with the top of the first paste state bed reactor 7；Coal tar fraction
Storage tank 2 is connected through the second valve 5 with the top of the first paste state bed reactor 7；The valve 9 of first paste state bed reactor, 7 top the 4th
It is connected with the top of the first vacuum filter 10；The bottom of first vacuum filter 10 is divided into two-way, surplus with solvent orange 2 A extraction absorption all the way
Remaining part storage tank 37 is connected, and another road is connected with the first silica gel phenol batcher 11；First silica gel phenol batcher 11 is exported and the second slurry
The top of state bed reactor 12 is connected；The bottom of solvent orange 2 A storage tank 3 is connected with solvent orange 2 A feed pump 6；The outlet of solvent orange 2 A feed pump 6 is divided into two
Road, is connected with the top of the first paste state bed reactor 7 all the way, another top of the valves 8 of Lu Jing tri- and the second paste state bed reactor 12
It is connected；The valve 13 of second paste state bed reactor, 12 top the 5th is connected with the second vacuum filter 14；Second vacuum filter
14 bottoms are divided into two-way, are connected all the way with the remaining part storage tank 37 of solvent orange 2 A extraction absorption, another road and the second silica gel phenol batcher 15
It is connected.
Referring to Fig. 2, the second silica gel phenol batcher 15 is connected through the 6th valve 17 with the top of the 3rd paste state bed reactor 20；It is molten
The bottom of agent B storage tanks 16 is connected with solvent B feed pumps 18, and the outlet of solvent B feed pumps 18 is divided into two-way, anti-with the 3rd slurry bed system all the way
The top of device 20 is answered to be connected, another valves 19 of Lu Jing seven are connected with the top of the 4th paste state bed reactor 25；3rd slurry reactor
The valve 21 of 20 top of device the 8th is connected with the top of the 3rd vacuum filter 22；The bottom of 3rd vacuum filter 22 is divided into two-way,
It is connected all the way with solvent B elution phenol storage tank 27, another silica gel phenol batchers 23 of Lu Yu tri- are connected；3rd silica gel phenol batcher 23
Outlet is connected with the top of the 4th paste state bed reactor 25；The valve 24 of 4th paste state bed reactor, 25 top the 9th and the 4th vacuum
Filter 26 is connected；The bottom of 4th vacuum filter 26 is divided into two-way, is connected all the way with solvent B elution phenol storage tank 27, Ling Yilu
It is connected with silica gel batcher 1.
Referring to Fig. 3, solvent B elution fractions storage tank 27 is connected with the entrance of solvent B elution fractions feed pump 28, and solvent B elution fractions are entered
The outlet of material pump 28 is connected with crude phenols knockout tower 29；The tower top of crude phenols knockout tower 29 and the top phase of crude phenols knockout tower overhead condenser 30
Even, the bottom of crude phenols knockout tower overhead condenser 30 is connected with the top of crude phenols knockout tower return tank of top of the tower 31；Crude phenols separate column overhead
The bottom of return tank 31 is connected with the entrance of crude phenols knockout tower overhead reflux pump 32, and the outlet of crude phenols knockout tower overhead reflux pump 32 is divided into two
Road, is connected with the tower top of crude phenols knockout tower 29 all the way, and another road is connected with solvent B storage tanks 16；The bottom of towe of crude phenols knockout tower 29 is divided into two
Road, is connected, i.e. crude phenols knockout tower tower bottom reboiler through crude phenols knockout tower tower bottom reboiler 33 with the bottom of towe of crude phenols knockout tower 29 all the way
33 gateways are connected with the bottom of towe of crude phenols knockout tower 29, and another road is connected with the crude phenols component discharging entrance of condenser 34；Crude phenols group
Separate the outlet of material condenser 34 with the entrance of crude phenols component discharging pump 35 to be connected, the outlet of crude phenols component discharging pump 35 and crude phenols storage tank 36
It is connected；The remaining part storage tank 37 of solvent orange 2 A extraction absorption is connected with the remaining entrance of part feed pump 38 of solvent orange 2 A extraction absorption, solvent orange 2 A extraction
The remaining outlet of part feed pump 38 of absorption is connected with neutral oil knockout tower 39；The top of neutral oil knockout tower 39 and neutral oil knockout tower tower
Push up the top of condenser 40 to be connected, the bottom of neutral oil knockout tower overhead condenser 40 and the top of neutral oil knockout tower return tank of top of the tower 41
It is connected；The bottom of neutral oil knockout tower return tank of top of the tower 41 is connected with the entrance of neutral oil knockout tower overhead reflux pump 42, neutral oil
It is divided into two-way from the outlet of column overhead reflux pump 42, is connected all the way with the top of neutral oil knockout tower 39, another road and solvent orange 2 A storage tank 3
It is connected；The bottom of towe of neutral oil knockout tower 39 is divided into two-way, all the way through neutral oil knockout tower tower bottom reboiler 43 and neutral oil knockout tower
39 bottom of towe are connected, i.e., the gateway of neutral oil knockout tower tower bottom reboiler 43 is connected with the bottom of towe of neutral oil knockout tower 39, Ling Yilu
It is connected with the neutral oil ingredient discharging entrance of condenser 44；Neutral oil ingredient discharging condenser 44 outlet and neutral oil ingredient discharging pump
45 entrances are connected, and the neutral outlet of oil ingredient discharging pump 45 is connected with neutral oil tank 46.
Coal tar fraction separating technology of the present utility model comprises the following steps：
First, solvent orange 2 A extraction absorption and solvent B elution processes flows
(1) solvent orange 2 A extraction and absorbing process flow
Referring to Fig. 1, coal tar fraction raw material is continuously stored up in coal tar fraction storage tank 2 by certain flow, then by coal tar
Oil distillate raw material injects the first paste state bed reactor 7.Solvent orange 2 A is heated to after 60~100 DEG C through solvent orange 2 A by solvent orange 2 A storage tank 3 simultaneously
Feed pump 6, which is pressurised into after 0.2~0.5MPa, to be pumped into the first paste state bed reactor 7.A certain amount of silica gel is by silica gel batcher 1 simultaneously
It is added in the first paste state bed reactor 7, the bottom of the first paste state bed reactor 7, which is passed through air, makes solvent orange 2 A, coal tar fraction raw material
Be well mixed with silica gel, control the temperature of the first paste state bed reactor 7 be 60~100 DEG C, extraction certain time after, by solvent orange 2 A with
Coal tar fraction raw material mixed liquor is separated through the first vacuum filter 10, and silica gel phenol is adopted through the outlet at bottom of the first vacuum filter 10
Go out, be added to by the first silica gel phenol batcher 11 in the second paste state bed reactor 12, and solvent orange 2 A remaining part of extraction absorption is by the
Another outlet at bottom outflow of one vacuum filter 10, is flowed in the remaining part storage tank 37 of solvent orange 2 A extraction absorption.It is added to the second slurry
The solvent orange 2 A that the silica gel phenol of bed reactor 12 is flowed into the second paste state bed reactor 12 through solvent orange 2 A feed pump 6 is washed.Gained
Mixed liquor is separated through the second vacuum filter 14, and outlet gained solvent orange 2 A extraction absorption in the bottom one of the second vacuum filter 14 is remaining
Part flows to the remaining part storage tank 37 of solvent orange 2 A extraction absorption, and another silica obtained phenol in outlet in the bottom of the second vacuum filter 14 is through second
Silica gel phenol batcher 15 carries out solvent B elution processes flows.Wherein, the volume ratio of coal tar fraction and solvent orange 2 A, silica gel is 1：1：
1~1：20：20；Solvent orange 2 A is the single alkane or the mixture (C5~C8 alkane of several single alkane in C5~C8 alkane
For n-alkane or branched paraffin).
(2) solvent B elution processes flow
Referring to Fig. 2, a certain amount of silica gel phenol is added in the 3rd paste state bed reactor 20 by the second silica gel phenol batcher 15, molten
After agent B is preheated to 20~60 DEG C through solvent B storage tanks 16, is flowed into after being forced into 0.2MPa~0.5MPa through solvent B feed pumps 18
The silica gel phenol added in the 3rd paste state bed reactor 20 is eluted in three paste state bed reactors 20, by the 3rd slurry reactor
The gained mixture of device 20 is separated through the 3rd vacuum filter 22, and gained eluting silica gel is through the bottom one of the 3rd vacuum filter 22
Outlet extraction, solvent B elution fractions are flowed out another outlet by the bottom of the 3rd vacuum filter 22, flow to solvent B elution fractions storage tank 27.
Gained eluting silica gel is added in the 4th paste state bed reactor 25 by the 3rd silica gel phenol batcher 23, and solvent B is fed through solvent B
Pump 18 is pumped into the 4th paste state bed reactor 25 and eluting silica gel is further eluted, and gained mixture passes through the 4th vacuum mistake
Filter 26 is separated, the bottom one of the 4th vacuum filter 26 export it is silica obtained recycled through silica gel batcher 1, the 4th is true
Solvent B elution fractions obtained by the empty another outlet in the bottom of filter 26 are flowed in solvent B elution fractions storage tank 27.
The solvent B is one or more of mixtures in ethyl acetate, toluene, ethanol, methanol.
2nd, the remaining part of solvent orange 2 A extraction absorption and solvent B elution fraction rectification process flows
(1) rectifying of solvent B elution fractions (crude phenols production) technological process
Referring to Fig. 3, the solvent B elution fractions from solvent B elution fractions storage tank 27 are preheating to after 20~60 DEG C to be eluted by solvent B
Part feed pump 28, which is forced into after 0.2~0.5MPa, enters the progress rectifying separation of crude phenols knockout tower 29.The tower top of crude phenols knockout tower 29 is produced
Go out solvent B steam, solvent B steam is all condensed into liquid phase through crude phenols knockout tower overhead condenser 30, and the solvent B after coagulating entirely enters
Crude phenols knockout tower return tank of top of the tower 31, is then back to through the part of crude phenols knockout tower overhead reflux pump 32 by certain reflux ratio
The tower top of crude phenols knockout tower 29, another part returns to solvent B storage tanks 16.
The crude phenols part of 29 outputs of crude phenols knockout tower is back to after the heating vaporization of crude phenols knockout tower tower bottom reboiler 33
In crude phenols knockout tower 29, another part is used as tower reactor product output.The crude phenols of output are cooled down through crude phenols component discharging condenser 34,
Crude phenols after cooling enter in crude phenols storage tank 36 through the pump of crude phenols component discharging pump 35 as product.
(2) remaining part rectifying (neutral oil production) technique of solvent orange 2 A extraction absorption
Referring to Fig. 3, the remaining part of solvent orange 2 A extraction absorption for extracting the remaining part storage tank 37 of absorption from solvent orange 2 A is preheating to 60~
It is pressurized to after 100 DEG C after 0.2~10MPa by the remaining part feed pump 38 of solvent orange 2 A extraction absorption and is pumped into neutral oil knockout tower 39 and carries out
Rectifying is separated.The tower top output solvent orange 2 A steam of neutral oil knockout tower 39, solvent orange 2 A steam separates column overhead complete condenser 40 through neutral oil
Liquid phase all is condensed into, the solvent orange 2 A after coagulating entirely enters in neutral oil knockout tower return tank of top of the tower 41, then through neutral oil knockout tower
The part of overhead reflux pump 42 is back to the tower top of neutral oil knockout tower 39 by certain reflux ratio, and another part returns to solvent orange 2 A
Recycled in storage tank 3.
The neutral oil part of 39 outputs of neutral oil knockout tower is heated through neutral oil knockout tower tower bottom reboiler 43 to be vaporized
After be back in neutral oil knockout tower 39, another part is used as tower reactor product output.The neutral oil ingredient of output is through the condenser that discharges
44 coolings, the neutral oil after cooling is pumped out through neutral oil ingredient discharging pump 45, and entering neutral oil tank 46 as product stores.
Solvent orange 2 A described in the utility model for single alkane or several single alkane in C5~C8 alkane mixing
Thing (C5~C8 alkane is n-alkane or branched paraffin).
The silica gel particle diameter is 75~250 μm, and silica gel is adsorbent.The bottom one of 4th vacuum filter 26 outlet gained silicon
Glue can be recycled through silica gel batcher 1.
The utility model can realize the continuous separation of coal tar, obtain neutral oil ingredient and crude phenols component, neutral oil
Component, crude phenols component are product.
Solvent orange 2 A enters in neutral oil knockout tower return tank of top of the tower 41, then through neutral oil knockout tower overhead reflux pump 42 1
Part is back to the tower top of neutral oil knockout tower 39 by certain reflux ratio, and another part, which returns to circulation in solvent orange 2 A storage tank 3, to be made
With.
Solvent B enters in crude phenols knockout tower return tank of top of the tower 31, then through the part of crude phenols knockout tower overhead reflux pump 32
The tower top of crude phenols knockout tower 29 is back to by certain reflux ratio, another part returns to solvent B storage tanks 16.It can be seen that, this practicality is new
The solvent orange 2 A and solvent B that type is obtained can be recycled.
The solvent orange 2 A feed pump moulding pressure scope is 0.2~0.5MPa, and feed temperature range is 60~100 DEG C.
The solvent B feed pump moulding pressures scope is 0.2~0.5MPa, and feed temperature range is 20~60 DEG C.
The remaining moulding pressure scope of part feed pump 38 of solvent orange 2 A extraction absorption is that 0.2~10MPa, temperature are 60~100
℃；
The moulding pressure scope of solvent B elution fractions feed pump 28 is 0.2~0.5MPa, and feed temperature range is 20~60
℃。
In order to illustrate effect of the present utility model, following examples are using low temperature coal in the progress of coal tar fraction separating technology
Tarry distillate separation test, in order to accurate Analyze ＆ separate product, using composition of the gas chromatograph-mass spectrometer (GC-MS) to product
Detected.Now divided using experimental raw to be derived from the coal tar (heavy oil) of semi-coke factory of northern Shensi Shenmu County as experimental subjects
From 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
Using the utility model coal tar fraction continuous separation technology, it (is specially C7 straight chain alkane that solvent orange 2 A is selected respectively
Hydrocarbon) and solvent B (be specially polar solvent ethyl acetate) be eluant, eluent, silica gel is adsorbent, the neutral oil in separation coal tar
Component, crude phenols component.
A certain amount of coal tar is taken to be tested according to foregoing schemes, after off-test and respectively to being obtained from products pot
Neutral oil ingredient and each 1mL of crude phenols component, then dissolved with 2mL dichloromethane, then carry out GC-MS analyses, analysis result
See Fig. 4, Fig. 5 and table 2 and table 3.
50g coal tar fractions are taken to be mixed with a certain amount of silica gel, the silica gel phenol obtained from the first vacuum filter is with molten
Agent A is eluted, and the use of the amount of solvent orange 2 A is every time 4L, elution number of times is respectively 1 time, 2 times, 3 times, 4 times, the neutrality obtained after elution
Oil detects that analysis result is as shown in Figure 6 by GC-MS.Can be obtained by Fig. 6, with elution number of times increase neutral oil in phenol content by
Decrescence few, when it is 3 times to elute number of times, phenol content is basically reached at least in neutral oil, and effect is eluted when elution number of times is more than 3 times
It is unobvious, and increase cost, consider, elution number of times is advisable for 3 times.Silica obtained phenol in second vacuum filter is passed through
Solvent B is eluted, and each solvent B elution amounts are also 4L, and elution number of times is respectively 1 time, 2 times, 3 times, 4 times, and what is obtained after elution is thick
Phenol detects that analysis result is as shown in Figure 7 by GC-MS.It can be obtained by Fig. 7, as solvent B is thick to the increase of silica gel phenol washing steps
Phenol content also gradually increases in phenol, when washing steps are 3 times, and phenol content basically reaches maximum in crude phenols, when washing steps are super
When crossing 3 times, DeGrain, and increase cost are eluted, is considered, washing steps are advisable when being 3 times.
Coalite tar neutral oil is constituted in table 2
Coalite tar crude phenols are constituted in table 3
The utility model has carried out product analysis to the peak of peak 1-26 in Fig. 4, to entering in Fig. 5 to peak number for 1-26 peak
Product analysis is gone, the peak number in figure has all been marked in table.
From Fig. 4, Fig. 5 and Fig. 6 experimental studies results, using coal tar fraction of the present utility model, continuously separation is new
Technique, can efficiently separate the neutral oil ingredient obtained in coal tar, crude phenols component, compared with conventional method, the utility model
A kind of method of the continuous separation coal tar of green, do not produce Industrial " three Waste " and the relatively conventional separator of device take up an area it is small,
Small investment, it is easily achieved industrialization.While the utility model overcomes, energy consumption present in existing coal tar processing process is big, grasp
The problems such as making numerous and diverse, low separation efficiency, pollution environment.
Claims (7)
1. a kind of coal tar fraction separator, it is characterised in that including the first paste state bed reactor (7) and the first vacuum filter
Machine (10), the first paste state bed reactor (7) top at the top of the first vacuum filter (10) with being connected, the first vacuum filter (10)
Bottom is divided into two-way, is connected all the way with the remaining part storage tank (37) of solvent orange 2 A extraction absorption, another road and the second paste state bed reactor
(12) top is connected, and the second paste state bed reactor (12) bottom is connected with the 3rd paste state bed reactor (20)；3rd slurry bed system is anti-
Answer device (20) top with being connected at the top of the 3rd vacuum filter (22), the 3rd vacuum filter (22) bottom is divided into two-way, all the way
It is connected with solvent B elution fractions storage tank (27), is connected at the top of another paste state bed reactors of Lu Yu tetra- (25)；Solvent B elution fractions are stored up
Tank (27) is connected with crude phenols knockout tower (29), and solvent orange 2 A extraction absorption remaining (37) is connected with neutral oil knockout tower (39).
2. a kind of coal tar fraction separator according to claim 1, it is characterised in that the second paste state bed reactor
(12) it is connected with the second vacuum filter (14), the second vacuum filter (14) bottom is divided into two-way, extracts inhale with solvent orange 2 A all the way
Attached remaining part storage tank (37) is connected, and is connected at the top of another paste state bed reactors of Lu Yu tri- (20).
3. a kind of coal tar fraction separator according to claim 1, it is characterised in that the 4th paste state bed reactor
(25) top is connected with the 4th vacuum filter (26)；4th vacuum filter (26) bottom is divided into two-way, is washed all the way with solvent B
De- part storage tank (27) is connected, and another road at the top of the first paste state bed reactor (7) with being connected.
4. a kind of coal tar fraction separator according to claim 1, it is characterised in that crude phenols knockout tower (29) tower top
With being connected at the top of crude phenols knockout tower overhead condenser (30), crude phenols knockout tower overhead condenser (30) bottom and crude phenols knockout tower tower
Push up and be connected at the top of return tank (31), crude phenols knockout tower return tank of top of the tower (31) bottom enters with crude phenols knockout tower overhead reflux pump (32)
Mouth is connected, and crude phenols knockout tower overhead reflux pump (32) outlet is divided into two-way, is connected all the way with crude phenols knockout tower (29) tower top, another
Road is connected with solvent B storage tanks (16).
5. a kind of coal tar fraction separator according to claim 1, it is characterised in that crude phenols knockout tower (29) bottom of towe
It is divided into two-way, is connected all the way through crude phenols knockout tower tower bottom reboiler (33) with crude phenols knockout tower (29) bottom of towe, another road and crude phenols
Component discharging condenser (34) entrance is connected, crude phenols component discharging condenser (34) outlet and crude phenols component discharging pump (35) entrance
It is connected, crude phenols component discharging pump (35) outlet is connected with crude phenols storage tank (36).
6. a kind of coal tar fraction separator according to claim 1, it is characterised in that neutral oil knockout tower (39) is pushed up
Portion at the top of neutral oil knockout tower overhead condenser (40) with being connected, neutral oil knockout tower overhead condenser (40) bottom and neutral oil
It is connected at the top of knockout tower return tank of top of the tower (41)；Neutral oil knockout tower return tank of top of the tower (41) bottom separates column overhead with neutral oil
Reflux pump (42) entrance is connected, and neutral oil knockout tower overhead reflux pump (42) outlet is divided into two-way, all the way with neutral oil knockout tower
(39) top is connected, and another road is connected with solvent orange 2 A storage tank (3).
7. a kind of coal tar fraction separator according to claim 1, it is characterised in that neutral oil knockout tower (39) tower
Bottom is divided into two-way, is connected all the way through neutral oil knockout tower tower bottom reboiler (43) with neutral oil knockout tower (39) bottom of towe, Ling Yilu
It is connected with neutral oil ingredient discharging condenser (44) entrance；Neutral oil ingredient discharging condenser (44) outlet goes out with neutral oil ingredient
Expect that pump (45) entrance is connected, neutral oil ingredient discharging pump (45) outlet is connected with neutral oil tank (46).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867556A (en) * | 2017-03-01 | 2017-06-20 | 西北大学 | A kind of coal tar fraction separating technology and device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867556A (en) * | 2017-03-01 | 2017-06-20 | 西北大学 | A kind of coal tar fraction separating technology and device |
| CN106867556B (en) * | 2017-03-01 | 2019-10-22 | 西北大学 | A kind of coal tar fraction separating technology and device |
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