CN107083256B - A kind of separation method of aromatic naphtha - Google Patents
A kind of separation method of aromatic naphtha Download PDFInfo
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- CN107083256B CN107083256B CN201610087634.4A CN201610087634A CN107083256B CN 107083256 B CN107083256 B CN 107083256B CN 201610087634 A CN201610087634 A CN 201610087634A CN 107083256 B CN107083256 B CN 107083256B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/02—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents with two or more solvents, which are introduced or withdrawn separately
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to oil and petroleum distillate manufacture fields, disclose a kind of separation method of aromatic naphtha, and this method includes：Aromatic naphtha is mixed with the first solvent, the first light solution phase and the first heavy solution phase are centrifugally separating to obtain through first；First weight solution is mutually washed using the second solvent, the second light solution phase and the second heavy solution phase are centrifugally separating to obtain through second；Second light solution is mutually washed using the first solvent, the light solution phase of third and third weight solution phase are centrifugally separating to obtain through third；It mixes the first light solution phase and the light solution of third to obtain light components, mixes the second heavy solution phase and third weight solution to obtain heavy component；First solvent is more than the solubility to few cycloaromatics to the solubility of condensed-nuclei aromatics, and the second solvent is more than the solubility of few cycloaromatics the solubility to condensed-nuclei aromatics.The method of the present invention improves few cycloaromatics and the separative efficiency of condensed-nuclei aromatics, comparable in environmental protection index, also improves the yield of environment-friendly type aromatic rubber oil, is conducive to improve processing performance and physical property of the sizing material in Oil feeding process.
Description
Technical field
The present invention relates to a kind of methods of the aromatics seperation in aromatic hydrocarbons oil product.
Background technology
Filling oil is one of primary raw material during rubber production, and appropriate addition can improve the plasticity of rubber, reduce rubber
The viscosity and melting temperature of glue, reduce the production cost of rubber.Rubber production and rubber product performance improvement are risen extremely important
Effect.Aromatic hydrocarbon rubber extender oil in filling oil have aromatic carbon content is high, density is big, viscosity is high, with polar rubber compatibility
The features such as good and processing performance is excellent is the excellent softening agent for producing tire and footwear product rubber.Produce the butylbenzene of tire
Rubber is that the atactic polymer of butadiene and styrene forms emulsion and carry out polymerisation and is prepared in water, polymerization process
The filling oil pole of middle addition is higher, and emulsifiability is better, degree of the dissolving each other rubber that is higher, therefore using of polymer and filling oil
Glue filling oil requires higher aromatic carbon content.Tyre rubber is filled in oil production process, and aromatic hydrocarbon rubber filling oil is general
Account for 30% or so of rubber quality.
Aromatic hydrocarbon rubber filling oil is generally urged by the tapped oil or heavy oil of solvent refining in production of lube base oils
Change cracking slurry oil to concoct, usually contains the polycyclic aromatic hydrocarbon of 10-30 weight %.Now with the increasingly strict of environmental regulation,
Polycyclic aromatic hydrocarbon is considered as organic pollution, and there is the aromatic hydrocarbon rubber that polycyclic aromatic hydrocarbon content is more than 3 weight % by shutting mechanism in European Union
Oil is classified as toxic substance.European Union signature instruction 2005/69/EC in 2005, the instruction clearly limit in aromatic hydrocarbon rubber filling oil
(polycyclic aromatic hydrocarbons, are abbreviated as benzo (a) pyrene (B (a) P) and eight kinds of carcinogenic condensed-nuclei aromatics
PAHs content), wherein B (a) P contents be not more than 1mg/kg, benzo (a) anthracene,Benzo (b) fluoranthene, benzo (k) fluoranthene,
Benzo (j) fluoranthene, benzo (a) pyrene, benzo (e) pyrene and the carcinogenic condensed-nuclei aromatics PAHs total contents of eight kinds of dibenzo (a, h) anthracene are little
In 10mg/kg.The DAE for meeting above-mentioned environmental protection index requirement is known as environment-friendly type aromatic hydrocarbon rubber extender oil (abbreviation environment-friendly aromatic oil).
Multinomial environment-friendly aromatic rubber oil production technology is announced both at home and abroad, for example, method disclosed in US6878263 is to use
The method production that the sedimentation of solvent refining Extract low temperature detaches again meets the aromatic hydrocarbon rubber filling oil of environmental protection index requirement.
Method disclosed in US6802960 is using furfural, phenol or N-Methyl pyrrolidone as solvent, using in two-stage extraction
The tapped oil of two stage extraction tower makees the aromatic hydrocarbon rubber filling oil that rubber filling oil production meets environmental protection index requirement.
For another example, CN101386688B discloses a kind of preparation method of aromatic rubber oil, and it is molten that this method, which includes with furfural,
Agent is once extracted feedstock oil in extraction tower, and top obtains raffinate, and lower part obtains extracting solution, and raffinate evaporation removes
Primary purification oil is obtained after removing furfural, primary purification oil is subjected to secondary extracting in extraction tower, top obtains raffinate, lower part
Extracting solution is obtained, raffinate evaporation obtains secondary fine liquefaction after removing furfural.This method is prepared into using the method extracted twice
To refined oil, and the aromatic hydrocarbon rubber filling oil for meeting environmental protection index is obtained after bleaching earth adsorption.
For another example, CN101906317B discloses a kind of method with preparing environment-friendly aromatic oil from catalytic cracking slurry oil, this method
Feedstock oil is extracted with polar solvent and alkane solvent, isolated upper solution mutually uses polar solvent to carry out 1- again
20 extractions, obtain the environmentally-frierubber rubber filling oil for meeting environmental requirement.
Using the density contrast of each component in solvent and feedstock oil and solvent to the poor solubility of different component in the above method
Different, the separation of different component is realized in contact of the progress feedstock oil with solvent continuously or discontinuously, is met environmental protection to produce and is referred to
Mark desired aromatic hydrocarbon rubber oil.But still have that solvent and feedstock oil contact effect are poor, and different component divides in the prior art
It is low from efficiency so that environment protection oil CA values are low, cannot completely separate environment-friendly type aromatic rubber oil ingredient from feedstock oil
Problem.Therefore, it is necessary to which the contact process and separation process to solvent extraction production environment-friendly rubber oil are improved.
Invention content
The purpose of the present invention is provide a kind of separation method of new aromatic naphtha in view of the above-mentioned drawbacks in the prior art.
To achieve the goals above, the present invention provides a kind of separation method of aromatic naphtha, wherein the method includes：It will
Aromatic naphtha is mixed with the first solvent, and the first light solution phase and the first heavy solution phase are centrifugally separating to obtain through first；By described first
Weight solution is mutually washed using the second solvent, and the second light solution phase and the second heavy solution phase are centrifugally separating to obtain through second；It will
The second light solution is mutually washed using the first solvent, is centrifugally separating to obtain the light solution phase of third through third and third weight is molten
Liquid phase；It mixes the described first light solution phase and the light solution of third to obtain light components, by the second weight solution phase and
Triple solution mix to obtain heavy component；
The aromatic naphtha is aromatic naphtha containing few cycloaromatics and condensed-nuclei aromatics of the boiling point more than 300 DEG C, wherein described few
The aromatic ring number of cycloaromatics is two hereinafter, the aromatic ring number of the condensed-nuclei aromatics is three or more；
Wherein, first solvent is to the solubility of condensed-nuclei aromatics more than the solvent of the solubility to few cycloaromatics, institute
It is the solvent being more than to the solubility of few cycloaromatics to the solubility of condensed-nuclei aromatics to state the second solvent.
The separation method of aromatic naphtha provided by the invention is using mixed once, centrifugation and washs, centrifuges twice
In conjunction with and realize the separation of different component in aromatic naphtha, to obtain two kinds of products, be respectively rich in the heavy of condensed-nuclei aromatics
Component and light components rich in few cycloaromatics.Specifically, the mixing in first solvent, separation enable to aromatic hydrocarbons
Condensed-nuclei aromatics in oil carries out crude separation with few cycloaromatics；Washing, separation in second solvent enable to the first weight
Few cycloaromatics in solution phase is further detached with condensed-nuclei aromatics realization；Washing, separation in first solvent can make
The few cycloaromatics obtained in the second light solution phase is further detached with condensed-nuclei aromatics realization, and the separative efficiency of each component is high, by
This prepares the product that disclosure satisfy that different requirements.Wherein, the heavy constituent for being rich in condensed-nuclei aromatics can be used as pitch blend component；
Light component rich in few cycloaromatics can be used as environment-friendly type aromatic rubber oil, and product benzo (a) the pyrene content is low, and benzo
(a) anthracene,Benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (j) fluoranthene, benzo (a) pyrene, benzo (e) pyrene and dibenzo (a,
H) total content of eight kinds of condensed-nuclei aromatics (PAHs) of anthracene is also low, disclosure satisfy that European Union 2005/69/EC instructions require, condensed-nuclei aromatics
Mass fraction is less than 3 weight %, and aromatic carbon content (CA) is more than 18 weight %, this hair comparable in environmental protection index
Bright method improves the yield of environment-friendly type aromatic rubber oil, is conducive to increase economic efficiency, and is conducive to improve glue
Expect processing performance and physical property in Oil feeding process.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Attached drawing is to be used to provide further understanding of the present invention, an and part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the process flow diagram of the separation method of aromatic naphtha provided by the invention.
Reference sign
The first pipelines of 1-；The second pipelines of 2-；3- mixers；4- third pipelines；The first whizzers of 5-；6- the 4th is managed
Line；The 5th pipelines of 7-；The 6th pipelines of 8-；The second whizzers of 9-；The 7th pipelines of 10-；The 8th pipelines of 11-；12- the 9th is managed
Line；13- third whizzers；The tenth pipelines of 14-；The 11st pipelines of 15-；The first solvent recovering systems of 16-；17- the 12nd
Pipeline；The second solvent recovering systems of 19-；The 13rd pipelines of 20-.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
According to the present invention, the separation method of the aromatic naphtha includes：Aromatic naphtha is mixed with the first solvent, through the first centrifugation
Isolated first light solution phase and the first heavy solution phase；The first weight solution is mutually washed using the second solvent, is passed through
Second is centrifugally separating to obtain the second light solution phase and the second heavy solution phase；Mutually the first solvent is used to carry out the described second light solution
Washing is centrifugally separating to obtain the light solution phase of third and third weight solution phase through third；Described first light solution phase and third is light
Solution mixes to obtain light components, mixes the described second heavy solution phase and third weight solution to obtain heavy component；
Wherein, the aromatic naphtha is aromatic naphtha containing few cycloaromatics and condensed-nuclei aromatics of the boiling point more than 300 DEG C, described few
The aromatic ring number of cycloaromatics is two hereinafter, the aromatic ring number of the condensed-nuclei aromatics is three or more；
Wherein, first solvent is to the solubility of condensed-nuclei aromatics more than the solvent of the solubility to few cycloaromatics, institute
It is the solvent being more than to the solubility of few cycloaromatics to the solubility of condensed-nuclei aromatics to state the second solvent.
It is to be separated as those skilled in the art's it is generally understood that when by centrifuging mixture of non soluble liquids
Liquid mixture obtains highdensity solvent phase under the influence of centrifugal force, in centrifuge outer rim, referred to as heavy solution phase；And
Centrifuge inner edge obtains the solution phase of low-density, referred to as light solution phase.
The present invention is not particularly limited the type of the aromatic naphtha, can be that existing various boiling points are more than 300 DEG C
And the aromatic naphtha containing saturated hydrocarbons, few cycloaromatics, condensed-nuclei aromatics and colloid simultaneously, for example, can be catalytic cracking fractionating tower
Tapped oil, vacuum distillate or the solvent that heavy oil, vacuum distillate or the solvent-deasphalted oils got rid of outside bottom are obtained through solvent refining
The dewaxed oil and vacuum distillate or solvent that the tapped oil that deasphalted oil is obtained through solvent refining is obtained through solvent dewaxing again are de-
At least one of the tapped oil that the dewaxed oil that coal tar is obtained through solvent dewaxing is obtained through solvent refining again.By vacuum distillate
Or solvent extraction, specially this field usually may be used in the method that solvent-deasphalted oils, solvent dewaxed oil carry out solvent refining
Well known to technical staff.The side that the vacuum distillate or solvent-deasphalted oils and solvent-refined oil (tapped oil) are dewaxed
Solvent dewaxing usually may be used in method, is specifically known to the skilled person, and therefore not to repeat here.Wherein, the decompression evaporates
Point oil can be Light lube oil, the line distillate that subtracts three, the line distillate that subtracts four, at least one of the line distillate etc. that subtracts five.
The aromatic naphtha and the first solvent are mixed to get mixed material by a kind of specific implementation mode according to the present invention
Method includes：Aromatic naphtha is carried out strength with the first solvent to mix, forms a mixture phase.When material mixes, the mixing
The liquidus temperature of object can be the mixing temperature of 20-60 DEG C, preferably 25-55 DEG C namely pending tapped oil and the first solvent
It can be 20-60 DEG C, preferably 25-55 DEG C.
A kind of specific implementation mode according to the present invention, by the mixture of the aromatic naphtha and the first solvent isolated
The method of one light solution phase and the first heavy solution phase includes：It is molten that mixture is formed to immiscible two under the influence of centrifugal force
Liquid phase, outer rim is the first heavy solution phase, and inner edge is the first light solution phase.When first centrifugation is centrifuged first
When being carried out in device, the liquidus temperature in first whizzer can be 20-60 DEG C, preferably 25-55 DEG C.
The present invention is not particularly limited the type and dosage of first solvent mixed with aromatic naphtha, as long as can
So that the condensed-nuclei aromatics and colloid in the aromatic naphtha are detached with few cycloaromatics.It is particularly preferred that described first is molten
Agent is at least one of furfural and N-Methyl pyrrolidone.In addition, the dosage of the dosage and aromatic naphtha of first solvent
Weight ratio can be (0.5-6):1, preferably (1-3):1.
A kind of specific implementation mode according to the present invention, the first weight solution is mutually washed using the second solvent,
The method of isolated second light solution phase and the second heavy solution phase includes：Under the action of the centrifugal force pass through the second solvent described
First heavy solution phase forms two immiscible solution phases, and outer rim is the second heavy solution phase, and inner edge is the second light solution phase.
When described second, which centrifuges, is carried out in the second whizzer, liquidus temperature in second whizzer can be with
It is 55-120 DEG C, preferably 65-100 DEG C.Also the temperature for mutually using the first weight solution the second solvent to be washed, detached
Degree can be 55-120 DEG C, preferably 65-100 DEG C.
The present invention is not particularly limited the type and dosage of washing the second solvent of the first weight solution phase, as long as can
So that few cycloaromatics in the first heavy solution phase realizes further washing, separation.Preferably, second solvent is
Lighter hydrocarbons, lighter hydrocarbons, C of the more preferable boiling point at 80-150 DEG C5-C14N-alkane and C5-C8At least one of cycloalkane.Its
In, the C5-C14The specific example of n-alkane include but not limited to：In pentane, n-hexane, normal heptane, normal octane etc.
At least one.The C5-C8The specific example of cycloalkane include but not limited to：Pentamethylene, hexamethylene, cyclooctane, cycloheptane
At least one of Deng.It is particularly preferred that second solvent be boiling point 110-130 DEG C of lighter hydrocarbons, normal heptane, normal octane,
At least one of hexamethylene and cycloheptane.In addition, the dosage of second solvent and the dosage of the described first heavy solution phase
Weight ratio can be (0.1-2.5):1, preferably (0.3-2):1.
In order to ensure the washing effect of the first heavy solution phase of second solvent pair, second solvent is preferably from centrifugation point
Outer rim from device enters, and by disperser, as micropore dispersion device is evenly dispersed, and ensures that end spray orifice keeps enough pressures
Power.Wherein, the disperser in the whizzer is known to those skilled in the art, and details are not described herein.
A kind of specific implementation mode according to the present invention, the described second light solution is mutually washed using the first solvent,
The method of the light solution phase of isolated third and third weight solution phase includes：Under the action of the centrifugal force pass through the first solvent described
Second light solution phase forms two immiscible solution phases, and outer rim is third weight solution phase, and inner edge is the light solution phase of third.
When third centrifugation carries out in third whizzer, the liquidus temperature in the third whizzer can be
30-70 DEG C, preferably 35-65 DEG C.That is, the described second light solution mutually to be used to the temperature that the first solvent is washed, detached
It can be 30-70 DEG C, preferably 35-65 DEG C.
The present invention is not particularly limited the type of the first solvent of the second light solution phase of the washing, as long as can make
It obtains the condensed-nuclei aromatics in the second light solution phase and realizes further washing, separation.It is particularly preferred that first solvent
For at least one of furfural and N-Methyl pyrrolidone.In addition, the dosage of first solvent and the described second light solution phase
The weight ratio of dosage can be (0.2-3):1, preferably (0.5-2.5):1.
Under preferable case, in order to easily facilitate separation, for the first solvent for mix with aromatic naphtha and for washing the
First solvent of the second light industry bureau solution phase selects identical solvent.
In order to ensure the washing effect of first the second light solution phase of solvent pair, first solvent is preferably from whizzer
Inner edge enter, and by disperser, as micropore dispersion device is evenly dispersed, and ensure that end spray orifice keeps enough pressure.Its
In, the disperser in the whizzer is known to those skilled in the art, and details are not described herein.
Usually, the step of aromatic naphtha being mixed using the first solvent, being centrifuged and by described first
Weight solution is mutually washed using the second solvent, centrifuges and mutually washed using the first solvent with by the described second light solution
The step of washing, centrifuging can carry out in Clothoid type centrifuge.In order to which centrifuge phase used will be centrifuged three times
Distinguish, will implement aromatic naphtha separation centrifuge be known as " the first whizzer ", by implement first weight solution phase separation from
Heart device is known as " the second whizzer ", and the centrifuge for implementing the second light solution phase separation is known as " third whizzer ".
In separation process, a kind of specific preferred embodiment according to the invention, the rotating speed of first whizzer can
Think 4000-5000rpm, preferably 4200-4800rpm；The rotating speed of second whizzer can be 3000-
4000rpm, preferably 3200-3800rpm.The rotating speed of the third whizzer can be 3500-4500rpm, preferably
3700-4300rpm.The above-mentioned rotating speed preferably centrifuged is respectively adopted during centrifuging three times, enables to
The separation of condensed-nuclei aromatics and few cycloaromatics is more abundant.
Aromatic hydrocarbons oil treatment process provided by the invention can operate continuously, can also intermittent operation.
The processing method of high aromatic oil provided by the invention is further described in detail below by attached drawing.
It is mixed as shown in Figure 1, feedstock oil is introduced into through the second pipeline 2 in mixer 3 through the first pipeline 1 and the first solvent, it
The first whizzer 5 is introduced by third pipeline 4, obtains the first light solution phase and the first heavy solution phase.First heavy solution phase
The second whizzer 9 is introduced through the 5th pipeline 7, the second solvent introduced through the 6th pipeline 8 washs, and obtains the second light solution phase
With the second heavy solution phase, the second light solution mutually introduces third whizzer 13 through the 8th pipeline 11, is introduced through the 9th pipeline 12
The washing of the first solvent, obtain the light solution phase of third and third weight solution phase.Second weight solution is mutually through the 7th pipeline 10 and third
Weight solution mutually through the 11st pipeline 15 mixing go in the first solvent recovering system 16 to remove the first solvent, after through the 12nd pipeline
17 extractions obtain condensed-nuclei aromatics oil (not marking the first solvent trend in Fig. 1).First light solution is mutually through the 4th pipeline 6 and third
Light solution mutually goes in the second solvent recovering system 19 to remove the second solvent through the mixing of the tenth pipeline 14, after through the 14th pipeline 20
Extraction obtains few cyclophane hydrocarbon ils (not marking the second solvent trend in Fig. 1).
The present invention will be further described in detail by specific embodiment below.
Embodiment 1
The embodiment is used to illustrate the separation method of aromatic naphtha provided by the invention.
Using low condensation point catalytic slurry as feedstock oil, property is shown in Table 1.It is handled according to the flow of Fig. 1, specific steps are such as
Under：Feedstock oil and solvent are introduced into the first whizzer after mixer mixes, the mass ratio of the first solvent and feedstock oil is
2:1, mixing temperature is 25 DEG C, and separation temperature is 25 DEG C, and the inner edge of the first whizzer obtains the first light solution phase, and outer rim obtains
To the first heavy solution phase.First weight solution mutually enters through the second whizzer inner edge, and the second solvent is through the second centrifuge outer rim
Into the mass ratio of the second solvent and the first weight solution phase is 1:1, wash temperature is 65 DEG C, washs and centrifuges through the second solvent
Separation, obtains the second heavy solution phase in the second centrifuge outer rim, the second light solution phase is obtained in inner edge.Second light solution is mutually through
Three whizzer outer rims enter, and the first solvent enters through third centrifuge inner edge, the matter of the first solvent and the second light solution phase
Amount is than being 0.6:1, wash temperature is 40 DEG C, washs and centrifuges through the first solvent, third is obtained in third centrifuge outer rim
Weight solution phase, the light solution phase of third is obtained in inner edge.It is 4200 turns/min, the second centrifugation point that first whizzer, which detaches rotating speed,
It is 3800 turns/min from device washing rotating speed, it is 3700 turns/min that third whizzer, which washs rotating speed,.Wherein, the first solvent is chaff
Aldehyde, the second solvent are hexamethylene.Second weight solution phase is mixed with third weight solution mutually goes the first solvent to return as weight solution
Solvent is removed in receipts system, obtains condensed-nuclei aromatics oil.First light solution phase is mixed with the light solution of third as light solution phase
It goes in the second solvent recovering system to remove solvent, obtains few cyclophane hydrocarbon ils.The production of the condensed-nuclei aromatics oil and few cyclophane hydrocarbon ils produced
Product yield and property are shown in Table 2.
Comparative example 1
The comparative example is used to illustrate the aromatic hydrocarbons oil treatment process of the prior art.
Feedstock oil is handled according to the method for embodiment 1, unlike, the first solvent is divided after being mixed with feedstock oil using sedimentation
From method, settling temperature is 25 DEG C, sedimentation time 100min.First weight solution phase is divided after being mixed with the second solvent using sedimentation
From method, mixing temperature is 65 DEG C, and settling temperature is 65 DEG C, sedimentation time 70min.Second light solution phase is mixed with the first solvent
It is 40 DEG C that sedimentation method for separating, mixing temperature are used after conjunction, and settling temperature is 40 DEG C, sedimentation time 70min.The condensed ring produced
The product yield and property of aromatic naphtha and few cyclophane hydrocarbon ils are shown in Table 2.
Embodiment 2
The embodiment is used to illustrate the separation method of aromatic naphtha provided by the invention.
To subtract three, line dewaxes tapped oil as feedstock oil, and property is shown in Table 1.It is handled according to the flow of Fig. 1, specific steps
It is as follows：Feedstock oil is introduced into the first whizzer, the mass ratio of the first solvent and feedstock oil with solvent after mixer mixes
It is 1.2:1, mixing temperature is 35 DEG C, and separation temperature is 35 DEG C, and the first whizzer inner edge obtains the first light solution phase, outer rim
Obtain the first heavy solution phase.First weight solution mutually through the second centrifuge inner edge enter, the second solvent through the second whizzer outside
Edge enters, and the mass ratio of the second solvent and the first weight solution phase is 2:1, wash temperature be 80 DEG C, through the second solvent wash and from
The heart detaches, and obtains the second heavy solution phase in the second whizzer outer rim, the second light solution phase is obtained in inner edge.Second light solution
Mutually enter through third centrifuge outer rim, the first solvent enters through third whizzer inner edge, the first solvent and the second light solution
The mass ratio of phase is 1.3:1, wash temperature is 35 DEG C, washs and centrifuges through the first solvent, outside third whizzer
Edge obtains third weight solution phase, and the light solution phase of third is obtained in inner edge.It is 4800 turns/min that first whizzer, which detaches rotating speed,
It is 3200 turns/min that second whizzer, which washs rotating speed, and it is 4300 turns/min that third whizzer, which washs rotating speed,.Wherein,
One solvent is furfural, and the second solvent is normal heptane.Second heavy solution phase is mixed with third weight solution and is mutually gone as weight solution
Solvent is removed in first solvent recovering system, obtains condensed-nuclei aromatics oil.First light solution phase and the light solution of third are mixed into work
It mutually goes in the second solvent recovering system to remove solvent for light solution, obtains few cyclophane hydrocarbon ils.The condensed-nuclei aromatics oil and few ring produced
The product yield and property of aromatic naphtha are shown in Table 2.
Comparative example 2
The comparative example is used to illustrate the aromatic hydrocarbons oil treatment process of the prior art.
Feedstock oil is handled according to the method for embodiment 2, unlike, the first solvent is divided after being mixed with feedstock oil using sedimentation
From method, settling temperature is 35 DEG C, sedimentation time 90min.First weight solution phase is divided after being mixed with the second solvent using sedimentation
From method, mixing temperature is 80 DEG C, and settling temperature is 80 DEG C, sedimentation time 50min.Second light solution phase is mixed with the first solvent
It is 35 DEG C that sedimentation method for separating, mixing temperature are used after conjunction, and settling temperature is 35 DEG C, sedimentation time 70min.The condensed ring produced
The product yield and property of aromatic naphtha and few cyclophane hydrocarbon ils are shown in Table 2.
Embodiment 3
The embodiment is used to illustrate the separation method of aromatic naphtha provided by the invention.
Using the dewaxed oil for the line tapped oil that subtracts four as feedstock oil, property is shown in Table 1.It is handled according to the flow of Fig. 1, specifically
Steps are as follows：Feedstock oil is introduced into the first centrifuge, the mass ratio of the first solvent and feedstock oil with solvent after mixer mixes
It is 2.5:1, mixing temperature is 55 DEG C, and separation temperature is 55 DEG C, and the first centrifuge inner edge obtains the first light solution phase, and outer rim obtains
First heavy solution phase.First weight solution mutually enters through the second centrifuge inner edge, and the second solvent enters through the second centrifuge outer rim, the
Two solvents and the mass ratio of the first weight solution phase are 1.5:1, wash temperature is 100 DEG C, is washed through the second solvent, in the second centrifugation
Device outer rim obtains the second heavy solution phase, and the second light solution phase is obtained in inner edge.Second light solution mutually through third centrifuge outer rim into
Enter, the first solvent enters through third centrifuge inner edge, and the mass ratio of the first solvent and the second light solution phase is 2:1, wash temperature
It is 65 DEG C, is washed through the first solvent, obtains third weight solution phase in third centrifuge outer rim, the light solution of third is obtained in inner edge
Phase.It is 4600 turns/min that first centrifuge, which detaches rotating speed, and it is 3600 turns/min that the second centrifuge, which washs rotating speed, and third centrifuge is washed
It is 4000 turns/min to wash rotating speed.Wherein, the first solvent is N-Methyl pyrrolidone, and the second solvent is normal octane.Second weight is molten
Liquid phase mixes with third weight solution and mutually goes in the first solvent recovering system to remove solvent as weight solution, obtains condensed-nuclei aromatics
Oil.First light solution phase is mixed with the light solution of third and mutually goes in the second solvent recovering system to remove solvent as light solution,
Obtain few cyclophane hydrocarbon ils.The product yield and property of the condensed-nuclei aromatics oil and few cyclophane hydrocarbon ils produced are shown in Table 2.
Embodiment 4
The embodiment is used to illustrate the separation method of aromatic naphtha provided by the invention.
Feedstock oil is handled according to the method for embodiment 3, unlike, it is 3700 turns/min that the first centrifuge, which detaches rotating speed,
It is 4300 turns/min that second centrifuge, which washs rotating speed, and it is 3000 turns/min that third centrifuge, which washs rotating speed,.The condensed-nuclei aromatics produced
The product yield and property of oil and few cyclophane hydrocarbon ils are shown in Table 2.
Table 1
Table 2
It can be seen from the results that the yield for the condensed-nuclei aromatics oil that the sedimentation method for separating of comparative example 1 and comparative example 2 obtains is equal
Higher, saturated hydrocarbons and single double ring arene mass fraction are respectively 19.9% and 43.3% in condensed-nuclei aromatics oil, are illustrated in aromatic naphtha
The separative efficiency of saturated hydrocarbons and single double ring arene is to be improved, while the yield of few cyclophane hydrocarbon ils is low.And the present invention is used to implement
The yield of the isolated few cyclophane hydrocarbon ils of the method for example 1 and embodiment 2 respectively reaches 9.4% and 34.6%, is above comparison
Example 1 and comparative example 2, while few cyclophane hydrocarbon ils aromatic carbon content is respectively 18.0% and 21.4%, benzo (a) pyrene content and eight kinds it is thick
Cycloaromatics (PAHs) meets requirement of the European Union 2005/69/EC instructions about tyre rubber oil, and polycyclic aromatic hydrocarbon mass fraction is equal
It is superior in quality environment-friendly rubber oil no more than 3 weight %.In addition, the condensed-nuclei aromatics oil that embodiment 1 and embodiment 2 obtain
Yield is low, and saturated hydrocarbons and single double ring arene mass fraction are less in condensed-nuclei aromatics oil, illustrate the good separating effect of different component.
By embodiment 4 and the first centrifuge it can be seen from the comparing result of embodiment 3 in currently preferred mix
Centrifugal rotational speed and twice wash when the second centrifuge and third centrifuge centrifugal rotational speed under the conditions of to aromatic naphtha carry out
Separation, separating effect is more preferably.
Either using the heavy oil got rid of outside catalytic cracking fractionating tower bottom as raw material it can be seen from the result of embodiment 1-4, with
Solvent refining tapped oil is raw material, or using the dewaxed oil of solvent refining tapped oil as raw material, and the method through the present invention can
Obtain the condensed-nuclei aromatics oil rich in condensed-nuclei aromatics and few cyclophane hydrocarbon ils rich in few cycloaromatics.Wherein, condensed-nuclei aromatics oil can be made
For pitch blend component；The aromatic carbon content of few cyclophane hydrocarbon ils is high, and benzo (a) pyrene mass fraction is not more than 1mg/kg, eight kinds of condensed ring
Aromatics quality score is not more than 10mg/kg, can be used as environment-friendly aromatic rubber oil, meet european union directive 2005/69/EC to tire
With the requirement of rubber oil.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, it can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (16)
1. a kind of separation method of aromatic naphtha, which is characterized in that the method includes：Aromatic naphtha is mixed with the first solvent, is passed through
First is centrifugally separating to obtain the first light solution phase and the first heavy solution phase；Mutually the second solvent is used to carry out the first weight solution
Washing, the second light solution phase and the second heavy solution phase are centrifugally separating to obtain through second；Described second light solution is mutually used first
Solvent is washed, and the light solution phase of third and third weight solution phase are centrifugally separating to obtain through third；By the described first light solution phase
It mixes to obtain light components with the light solution of third, mixes the described second heavy solution phase and third weight solution to obtain heavy group
Point；
The aromatic naphtha is aromatic naphtha containing few cycloaromatics and condensed-nuclei aromatics of the boiling point more than 300 DEG C, wherein few cyclophane
The aromatic ring number of hydrocarbon is two hereinafter, the aromatic ring number of the condensed-nuclei aromatics is three or more；
First solvent is to the solubility of condensed-nuclei aromatics more than the solvent of the solubility to few cycloaromatics, second solvent
To be more than the solvent to the solubility of condensed-nuclei aromatics to the solubility of few cycloaromatics；
First centrifugation carries out in the first whizzer, and the liquidus temperature in first whizzer is
20-60℃；The rotating speed of first whizzer is 4000-5000rpm；
Second centrifugation carries out in the second whizzer, and the liquidus temperature in second whizzer is
55-120℃；The rotating speed of second whizzer is 3000-4000rpm；
The third centrifugation carries out in third whizzer, and the liquidus temperature in the third whizzer is
30-70℃；The rotating speed of the third whizzer is 3500-4500rpm.
2. according to the method described in claim 1, wherein, the weight ratio of first solvent and aromatic naphtha is 0.5-6:1.
3. according to the method described in claim 2, wherein, the weight ratio of first solvent and aromatic naphtha is 1-3:1.
4. according to the method described in claim 1, wherein, the weight ratio of first solvent and the second light solution phase is 0.2-3:
1。
5. according to the method described in claim 4, wherein, the weight ratio of first solvent and the second light solution phase is 0.5-
2.5:1。
6. according to the method described in any one of claim 1-5, wherein for the first solvent for being mixed with aromatic naphtha and
The first solvent for washing the second light solution phase is each independently at least one of furfural and N-Methyl pyrrolidone.
7. according to the method described in claim 6, wherein, the first solvent for mix with aromatic naphtha and for washing second
First solvent of light solution phase selects identical solvent.
8. according to the method described in claim 1, wherein, the liquidus temperature in first whizzer is 25-55 DEG C；Institute
The rotating speed for stating the first whizzer is 4200-4800rpm.
9. according to the method described in claim 1, wherein, the weight ratio of second solvent and the first heavy solution phase is 0.1-
2.5:1。
10. according to the method described in claim 9, wherein, the weight ratio of second solvent and the first heavy solution phase is 0.3-
2:1。
11. according to the method described in claim 1,9 or 10, wherein second solvent be boiling point 80-150 DEG C lighter hydrocarbons,
C5-C14N-alkane and C5-C8At least one of cycloalkane.
12. according to the method for claim 11, wherein second solvent is lighter hydrocarbons of the boiling point at 110-130 DEG C, positive heptan
At least one of alkane, normal octane, hexamethylene and cycloheptane.
13. according to the method described in claim 1, wherein the liquidus temperature in second whizzer is 65-100
℃；The rotating speed of second whizzer is 3200-3800rpm.
14. according to the method described in claim 1, wherein, the liquidus temperature in the third whizzer is 35-65 DEG C；
The rotating speed of the third whizzer is 3700-4300rpm.
15. according to the method described in claim 1, wherein, the method further includes by the described first light solution phase and third
Before or after light solution mixes, solvent therein is removed, and the described second heavy solution phase and third are weighed into solution phase
Before or after mixing, solvent therein is removed.
16. according to the method described in claim 1, wherein, the aromatic naphtha is the heavy oil got rid of outside catalytic cracking fractionating tower bottom, subtracts
Tapped oil, vacuum distillate or the solvent-deasphalted oils that pressure distillate or solvent-deasphalted oils are obtained through solvent refining are through solvent essence
The dewaxed oil and vacuum distillate or solvent-deasphalted oils that the tapped oil being made is obtained through solvent dewaxing again are through solvent dewaxing
At least one of the tapped oil that obtained dewaxed oil is obtained through solvent refining again；Wherein, the vacuum distillate is second line of distillation
Distillate, the line distillate that subtracts three, the line distillate that subtracts four and at least one of the line distillate that subtracts five.
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| WO2013140272A1 (en) * | 2012-03-23 | 2013-09-26 | Indian Oil Corporation Ltd. | A process for manufacturing of rubber process oils with extremely low carcinogenic polycyclic aromatics compounds |
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| CN102220164A (en) * | 2010-04-15 | 2011-10-19 | 中国石油化工股份有限公司 | Utilization method of aldehydic water of furfural extraction solvent recovery system |
| CN102311776A (en) * | 2010-07-09 | 2012-01-11 | 中国石油化工股份有限公司 | Method for preparing aromatic rubber oil |
| CN102653686A (en) * | 2011-03-03 | 2012-09-05 | 中国石油化工股份有限公司 | Preparation method of aromatic rubber oil |
| WO2013140272A1 (en) * | 2012-03-23 | 2013-09-26 | Indian Oil Corporation Ltd. | A process for manufacturing of rubber process oils with extremely low carcinogenic polycyclic aromatics compounds |
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