CN103012045B - The method of adsorption separation of m-Xylene from C8 aronmatic - Google Patents

The method of adsorption separation of m-Xylene from C8 aronmatic Download PDF

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CN103012045B
CN103012045B CN201110290155.XA CN201110290155A CN103012045B CN 103012045 B CN103012045 B CN 103012045B CN 201110290155 A CN201110290155 A CN 201110290155A CN 103012045 B CN103012045 B CN 103012045B
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xylene
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strippant
desorption
aronmatic
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CN103012045A (en
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王辉国
马剑锋
王德华
郁灼
王志光
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Abstract

A kind of method of compartment dimethylbenzene from C8 aronmatic, be included in the C8 aronmatic mixture containing m-xylene and adsorbent contact under liquid phase state, m-xylene is formed Adsorption Phase by adsorbent, with the m-xylene in strippant desorption Adsorption Phase, obtain the Extract comprising strippant and m-xylene, rectifying Extract obtains m-xylene, position alkyl toluene between described strippant is selected from, and alkyl is wherein C 2~ C 4alkyl, this method can effectively improve desorption efficiency, reduces the energy consumption of adsorption separation process.

Description

The method of adsorption separation of m-Xylene from C8 aronmatic
Technical field
The present invention is a kind of method of a certain isomer of fractionation by adsorption from aromatic hydrocarbons mixture, specifically, is a kind of method of adsorption separation of m-Xylene from C8 aronmatic mixture.
Background technology
M-xylene (MX) is important basic organic chemical industry raw material, is widely used in the numerous areas such as synthetic resins, agricultural chemicals, medicine, coating and dyestuff.Highly purified m-xylene normally obtains from containing being separated ethylbenzene, p-Xylol, m-xylene and the mixed C 8 aromatics of o-Xylol.Because between four kinds of C8 aronmatic isomer, boiling point is close, conventional rectifying mode is adopted to be difficult to be separated, so the technique of compartment dimethylbenzene mainly contains several process forms such as sulfonation hydrolysis, Separation by Complexation, extractive distillation and fractionation by adsorption.Wherein sulfonation hydrolysis process production process discharges a large amount of spent acid contaminate environment, and Separation by Complexation technique uses HF-BF 3etching apparatus, extractive distillation needs to add extraction solvent in material to be separated, and often because of the purity that the selectivity of extraction solvent makes m-xylene product be difficult to reach very high not.Absorption method industrially realizes one of effective ways be separated between isomers, compared with traditional technology, it is pollution-free that adsorption method of separation has environmental friendliness, corrosion-free equipment manufacturing cost is low, product purity, yield are high, the advantages such as sorbent material long service life are the main development directions of compartment dimethylbenzene technology.
The realization of adsorption separation process comprises three key elements, and one is the zeolite adsorbents of excellent property; Two is the strippants matched with performance of the adsorbent; Three is suitable process forms.Continuous countercurrent simulated moving bed technology be develop up to now the most successful, most widely used a kind of adsorptive separation technology, be disclosed in US2985589 and US3201491, for the adsorption separation process of 5A zeolite to branched paraffin and straight-chain paraffin, large-scale application is in p-Xylol fractionation by adsorption subsequently, and progressively the process form becoming a kind of maturation is improved in development.Douglas M.Ruthven at Chemical Engineering Science, 1989, in 44 (5): 1011 ~ 1038, its principle, development course and commercial run are summed up.Thus, the study hotspot that new adsorption-desorption system becomes exploitation fractionation by adsorption novel method is found.
In prior art, the method for adsorption separation of m-Xylene mainly adopts NaY zeolite as sorbent material, and toluene is as strippant.The Y zeolite in exchangeable cation site is occupied as sorbent material using sodium ion as open in US4306107, toluene is as strippant, controlling sorbent material igloss water-content at 500 DEG C is 2% ~ 7%, by simulated moving bed technology adsorption separation of m-Xylene under 20 ~ 250 DEG C with normal pressure to 35 bar, maintenance liquid-phase condition.
The Y zeolite that CN1050595C and US5382747 proposes to be occupied using exchangeable cation position by sodium and lithium ion is simultaneously as sorbent material, controlling its igloss water-content at 500 DEG C is 1.5% ~ 3%, adsorption operations thermal creep stress between 100 ~ 150 DEG C, using toluene or indane as strippant.
It is that the NaY zeolite of 4 ~ 6 is as the application of m-xylene sorbent material that US5900523 describes silica/alumina molar ratio.During using toluene as strippant, it is 1.5% ~ 2% that sorbent material water-content controls, and during using indane as strippant, it is 1.5% ~ 2.5% that sorbent material water-content controls.
CN1939883A is that the Y zeolite of 5 ~ 6 is as sorbent material using silica/alumina molar ratio, adopt tetraline as strippant adsorption separation of m-Xylene from C8 aronmatic isomer, requiring that sorbent material water-content controls is 0 ~ 8%, and adsorption temp is 25 ~ 250 DEG C.
In adsorptive separation technology, following principle is followed in the selection of strippant usually: one is have good mutual solubility between material to be separated; Two is that stable in properties not easily chemical reaction occurs, in order to avoid cause undesirable consumption or make sepn process more complicated; Three is have enough boiling-point differences between material to be separated, so that by simple rectifying recycle and reuse; Four is have suitable adsorption strength on the sorbent, can displace the object product in Adsorption Phase, can not hinder the absorption of next cycle object product again and reduce zeolite efficiency because of the strong adsorption of self with rational mass flow rate.
Though the adsorption separating method proposed in prior art can realize m-xylene from the separation other arene isomer mixture flow, still have some deficits part.As using toluene as strippant, because its adsorptive power is relatively weak, the flow that the desorption completing m-xylene needs is comparatively large, and when follow-up rectifying, lower boiling toluene will reclaim from rectifying tower top, this will cause the increase of steam output, economical not in facility investment and energy consumption.Adopt the tetraline of heavy to make the deficiency that strippant compensate for toluene to a certain extent, but its adsorptive power is excessively strong, and sorbent material is reduced the adsorption efficiency of m-xylene.
Summary of the invention
The object of this invention is to provide a kind of method of adsorption separation of m-Xylene from C8 aronmatic, this method, by using special strippant, can effectively improve desorption efficiency, reduces the energy consumption of adsorption separation process.
The method of adsorption separation of m-Xylene from C8 aronmatic provided by the invention, be included in the C8 aronmatic mixture containing m-xylene and adsorbent contact under liquid phase state, m-xylene is formed Adsorption Phase by adsorbent, with the m-xylene in strippant desorption Adsorption Phase, obtain the Extract comprising strippant and m-xylene, rectifying Extract obtains m-xylene, position alkyl toluene between described strippant is selected from, and alkyl is wherein C 2~ C 4alkyl.
Between the present invention adopts, position alkyl toluene is strippant, to have an appointment the boiling-point difference of 40 DEG C with m-xylene (boiling point is 139.3 DEG C), than toluene (boiling point is 110.8 DEG C) as strippant, the rectifying being separated strippant after can making absorption is more prone to, significantly reduce the consumption of strippant, and significantly reduce the energy consumption of adsorption separation process.
Embodiment
In simulated moving bed adsorption lock out operation, the complexity that the circular flow of strippant and being realized by rectifying is separated from each other between feed composition, the importance weighing plant energy consumption, so strippant performance is one of important factor affecting device technique economy.
The present invention adopt two substituted alkyls on phenyl ring be between the aromatic hydrocarbons of position arrangement be the strippant of m-xylene fractionation by adsorption, the adsorption separation process being strippant than toluene has clear superiority.First, the strippant that the present invention adopts and m-xylene are had an appointment the boiling-point difference of 40 DEG C, and during using toluene as strippant, toluene differs 28.5 DEG C with the boiling point of m-xylene, and toluene flux required under normal running is approximately four times of raw material volume, when follow-up rectifying, a large amount of toluene will steam from tower top, obviously economical not in energy consumption.Adopt the inventive method heavy arene used as strippant, when rectifying separation strippant, strippant is discharged at the bottom of rectifying tower, and the C8 aronmatic that relative discharge is less distillates from tower top, and rectifying steam output can be made to reduce, and energy consumption reduces.
The present invention's strippant used is the toluene of the substituted alkyl having carbon number lower, and described alkyl is positioned at position between methylbenzyl, and described alkyl is selected from ethyl, propyl group or butyl.The preferred m-isopropyl toluene of position alkyl toluene or m-n-propyl toluene between described.
Sorbent material used in the inventive method is selected from y-type zeolite, and in its skeleton, the mol ratio of silicon oxide and aluminum oxide is 4.6 ~ 6.0, preferably 5.0 ~ 5.6.The outer exchangeable cation position of zeolite framework is that sodium ion or at least 80% is occupied by sodium ion, all the other are occupied by the IA race metal ion except sodium ion or IIA race metal ion, the described preferred Li of IA race metal ion except sodium +, the preferred Sr of IIA race metal ion 2+, namely described sorbent material is NaY zeolite, LiNaY zeolite or SrNaY zeolite, wherein Na +by Li +or Sr 2+the molar percentage exchanged, namely exchange degree is 4 ~ 15%.
For increasing the rate of mass transfer of sorbent material, the y-type zeolite of the preferred little crystal grain of sorbent material of the present invention, its average crystal grain particle diameter preferably 0.1 ~ 2.0 micron, more preferably 0.2 ~ 1.0 micron.
The water-content of sorbent material has a significant effect to adsorption selectivity, and in order to obtain good separating effect, should control sorbent material in operation has suitable water-content.In the inventive method, the water-content of sorbent material represents with the igloss amount of 600 DEG C of roastings after 2 hours, and sorbent material is 1 ~ 6 quality % in the igloss amount of 600 DEG C of roastings after 2 hours, preferably 2 ~ 4 quality %.
Industrial zeolite is generally Powdered, for ease of application, zeolite powder need be agglomerated into particulate matter with suitable processing method, coalescently shapingly can to carry out according to various technology well-known to those skilled in the art, after zeolite powder is mixed with binding agent, adopt the methods such as extrusion, compressing tablet, rolling balling coalescent shaping, consider from the hydromeehanics of sorbent material filling and use procedure, preferred coalescent molding mode is rolling balling.
The adsorption separation process of m-xylene of the present invention preferably operates under liquid phase state, consider from absorption angle merely, low temperature is favourable, but low temperature is unfavorable for that mass transfer spreads, rational selection is seeking balance point between absorption and mass transfer, based on this, the service temperature of adsorption separation of m-Xylene of the present invention is defined as 100 ~ 200 DEG C, preferably 140 ~ 180 DEG C, the object of Controlling System pressure ensures to make fluid be in full liquid phase state at the operational, and fractionation by adsorption pressure is 0.2 ~ 2.0MPa, preferably 0.4 ~ 1.2MPa.
Desorption utilizes strippant, cemented out by the object product m-xylene be adsorbed in sorbent material.After desorption, also need the Extract logistics to desorption process is collected to carry out rectifying, m-xylene is separated with strippant, reclaim m-xylene as product, strippant then recycles.Adsorb remaining poor MX logistics as raffinate also containing certain density strippant, recycled by rectifying separation strippant, C8 aronmatic in poor MX logistics can regenerate by isomerization reaction the mixed isomers comprising MX again, and the raw material as absorption continues to be separated m-xylene wherein.
For reaching required product purity, realize the continuous operation of industrial separation device, the sepn process of m-xylene and other C8 aronmatic isomer should be carried out having in multiple adsorbent bed simulation moving-bed device, described multiple be adsorbent bedly at least divided into absorption, purification, desorption three regions, preferably simulation moving-bed adsorbent bed absorption, purification, desorption and isolation four districts of being divided into carried out fractionation by adsorption operation.
Having in multiple adsorbent bed simulation moving-bed device, sorbent material is seated in pillar container as a fixed bed, adsorbent bed can be the series connection of multiple adsorption column, also can be divided into multiple bed in adsorption column inside by screen cloth or grid, liquid stream be communicated with from top to bottom between adsorbent bed, flows.Sorbent material maintains static, each adsorption column or adsorbent bedly connect at least one logistic pipeline, in order to inject or to extract the different logistics of adsorption separation process out, the different logistics of periodic variation from top to bottom enters or discharges adsorbent bed position, thus reach downward liquid flow in adsorption bed, the effect of the liquid-solid two-phase move counter-current simulation movement that sorbent material moves upward.The bed space of filled with adsorbent is referred to as adsorption chamber, and whole adsorption chamber is injected into or the different logistics of withdrawing device is divided at least three regions, and the m-xylene in mixing raw material completes absorption, purification, desorption process respectively in different regions.
During fractionation by adsorption operation, the C8 aronmatic mixture flow comprising m-xylene enters the adsorption zone of adsorption chamber, contact with zeolite adsorbents, Y zeolite has the characteristic of Preferential adsorption meta-isomer, enter in the geode of zeolite so the m-xylene in raw material is preferentially adsorbed, form Adsorption Phase, also have a small amount of non-MX impurity composition simultaneously and adsorbed; Sorbent material moves up and enters purification section, and the top-down mixture be made up of strippant and high purity MX fails to be convened for lack of a quorum a small amount of impurity adsorbed in progressively displacement sorption agent, and the MX of Adsorption Phase is progressively purified; Last at desorption district injection strippant, out, extracted out obtain Extract from adsorption chamber by the desorption from sorbent material of the MX through purifying, rectifying Extract recovery m-xylene, so can obtain the m-xylene product that purity is equal to or greater than 99.5 quality %.Adsorb remaining poor MX logistics to draw in addition from adsorption unit as raffinate, wherein also containing certain density strippant, strippant is gone out by rectifying separation, recycle together with the strippant of Extract rectifying separation, C8 aronmatic in poor MX logistics can regenerate by isomerization reaction the mixed isomers comprising MX again, and the raw material as absorption continues to be separated m-xylene wherein.
Adsorption selectivity and be weigh two important indicators of adsorbent separation performance quality to the Adsorption and desorption speed of extraction components.
When adsorption selectivity is for reaching adsorption equilibrium, the ratio of the quality of two components or the ratio of volume and the quality of these two kinds of components in fluid phase or the ratio of volume in Adsorption Phase.Described adsorption equilibrium refers to C 8after aromatic hydrocarbons and adsorbent contact, between Adsorption Phase and fluid phase, there is not state during component net transfer.Adsorption selectivity β is calculated by following formula:
β = A C / A D U C / U D
In formula, C with D represents for carrying out the two kinds of components be separated, A cand A drepresent respectively C, D in Adsorption Phase two component quality or volume ratio, U cand U drepresent respectively C, D in fluid phase two component quality or volume ratio.As the selectivity β ≈ 1.0 of two kinds of components, they are adsorbed or not almost identical by the degree of adsorbing each other, there is not the Preferential adsorption of wherein a kind of component.When β is greater than or less than 1.0, namely there is the sepn process that wherein a kind of component is preferentially adsorbed.Specifically, as β > 1.0, sorbent material is to component C Preferential adsorption, and as β < 1.0, sorbent material is to D component Preferential adsorption.Consider from the complexity be separated, extraction components is all the other components relatively, and β value is larger, and fractionation by adsorption is more easily carried out.And Adsorption and desorption speed faster, the circulation consumption of sorbent material and strippant can be reduced, improve product yield, reduce the process cost of adsorption separation device.Under the condition that sorbent material is determined, the adsorption selectivity of strippant character on feed composition and the Adsorption and desorption speed on extraction components all have remarkably influenced.
When the inventive method uses a kind of dynamic pulse test device to measure use different strippant, the selectivity of fractionation by adsorption system and the speed of Adsorption and desorption m-xylene.
This device is made up of feed system, adsorption column, electrical heater and pressure controlled valve etc.Adsorption column is the Stainless Steel Coil of φ 8 × 1 × 1800 millimeters, sorbent material loading amount 50 milliliters, is placed in temperature automatically controlled vertical electric furnace and heats.Adsorption column lower inlet is connected with nitrogen system with charging, and upper end outlet connects voltage-controlled valve and is connected with effluent collector.Test and be raw materials usedly the desorption liquid and pulse liquid (being equivalent to fractionation by adsorption raw material) prepared according to a certain percentage, desorption liquid consists of the strippant (D) of 30 volume % and the normal heptane (for thinner) of 70 volume %; Pulse liquid consists of ethylbenzene (EB), p-Xylol (PX), m-xylene (MX), o-Xylol (OX), the n-nonane (NC that content is respectively 5 volume % 9) and the desorption liquid of 75 volume %.
C 8between aromatic component, the mensuration process of adsorption selectivity is: load weighted sorbent material is loaded adsorption column concussion and tamp, and in 180 ~ 300 DEG C of dehydration activation in nitrogen gas stream, controls to keep suitable water-content in sorbent material.Then pass into the gas in desorption liquid removal system, pressure is risen to 0.8MPa, temperature rises to 160 DEG C, stop pass into desorption liquid, by 1.0 time -1volume space velocity pass into the pulse liquid of 8 milliliters, then change unconventional attached liquid and carry out wash-out with same air speed, within every 2 minutes, getting an elution samples, form with gas chromatographic analysis.With wash-out desorption liquid feed volume for X-coordinate, NC 9be ordinate zou with each concentration of component of EB, PX, MX, OX, the concentration curve of above-mentioned each component can be drawn out.As the NC of tracer agent 9do not adsorbed, first gone out peak, which gived the dead volume of adsorption system.Using the mid point of tracer agent peak width at half height as zero point, measure the net retention volume V of EB, PX, MX, OX each component peak width at half height mid point to zero point r, the net retention volume of any component is directly proportional to partition ratio during adsorption equilibrium, it reflects the situation of Isomers adsorption equilibrium, and the ratio of two component net retention volumes is adsorption selectivity β value, is also referred to as separation factor.
In order to the circulation realizing sorbent material uses continuously, the selectivity between extraction components and strippant is also important performance index, and the further parsing can testing the concentration curve of extraction components by paired pulses is here determined.When MX concentration in the front end effluent liquid of the pulsing concentration change curve of MX is risen to 90% from 10%, required desorption liquid volume is defined as adsorption rate [S a] 10-90, when concentration curve rear end MX concentration is dropped to 10% from 90%, required desorption liquid volume is defined as desorption rate [S d] 90-10.Ratio [the S of the two d] 90-10/ [S a] 10-90be defined as the adsorption selectivity β between MX and strippant mX/D.If β mX/Dbe less than 1.0 expression sorbent materials to be eager to excel to the selectivity of strippant, this is disadvantageous to adsorption process, if β mX/Dmuch larger than 1.0, then represent that the adsorptive power of strippant is too weak, desorption process will be made to become difficulty, and desirable situation is ratio beta mX/Dto equal or slightly larger than 1.0.
Between strippant with extraction components, the peak width at half height of the concentration curve that the mass transfer velocity of phase double replacement can be obtained by pulse testing characterizes, and peak width at half height numerical value is less, shows that mass transfer velocity is faster.Less peak width at half height can also reduce the overlapping degree of concentration curve between each component, reaches better separating effect.Strippant can be characterized by the net retention volume in pulse testing the desorption rate of extraction components.For the sorbent material of an industrial application, under the prerequisite meeting separating effect, wish, to extraction components, there is desorption rate faster, because the consumption of strippant can be reduced like this, more reasonable economically.
Further illustrate the present invention below by example, but the present invention is not limited to this.
Example 1
Investigate adsorption selectivity when m-isopropyl toluene makes strippant and the Adsorption and desorption speed to m-xylene.
Sorbent material is NaY zeolite bead, and Sinopec catalyzer Chang Ling branch office produces, and small spherical particles diameter 0.35 ~ 0.80 millimeter, the silica/alumina molar ratio in Y zeolite skeleton is 5.32, average crystal grain particle diameter 0.8 micron.Sorbent material initial moisture content 15 quality %, at 250 DEG C, in the nitrogen gas stream of 25L/h dry 2 hours before test, it is 3.5 quality % that 600 DEG C of roastings measure its igloss amount for 2 hours.
Desorption liquid is made up of the normal heptane of isopropyl toluene and 70 volume % between 30 volume %; Pulse liquid by content be respectively the n-nonane of 5 volume %, the desorption liquid of ethylbenzene, p-Xylol, m-xylene, o-Xylol and 75 volume % forms.
In adsorption column, first inject desorption liquid exhaust during on-test, heat up, Controlling System pressure is 0.8MPa, treat that temperature rises to 160 DEG C, when effluent liquid composition forms identical with fresh desorption liquid, sorbent material is desorbed that agent is saturated reaches balance, at this moment suspend and inject desorption liquid, switch adsorption column charging, with 1.0h -1air speed injects 8 milliliters of pulse liquids, then refills desorption liquid, continues with 1.0h -1the pulse liquid that injects of air speed drip washing, within every 2 minutes, get a desorption sample, stratographic analysis sample composition, draw each concentration of component change curve of recording of pulse testing, calculate separation factor, MX peak width at half height and net retention volume, the results are shown in Table 1.
Example 2
Investigate adsorption selectivity when m-isopropyl toluene makes strippant and the Adsorption and desorption speed to extraction components.
(1) sorbent material is prepared
NaY zeolite bead strontium ion used for example 1 is exchanged, exchange the strontium chloride aqueous solution that liquid is 0.07moL/L, Gu the liquid/volume ratio of strontium chloride solution used and NaY zeolite bead is 5: 1,92 DEG C, 0.1MPa, carry out strontium ion under agitation condition and exchange 6 hours.After exchange completes, filter exchange mother liquor, can't detect Cl with in deionized water wash to washings -1.After x-ray fluorescence spectrometry ion-exchange in sorbent material containing strontium oxide 2.81 quality %, sodium oxide 10.43 quality %, the mol ratio of sodium oxide and strontium oxide is 6.2: 1, and the molar percentage that sodium ion is exchanged by strontium ion and exchange degree are 13.9%.
(2) strippant performance is tested
By the SrNaY bead after ion-exchange in 230 DEG C of nitrogen gas stream dry 2 hours, it was 2.9 quality % that 600 DEG C of roastings measure its igloss amount for 2 hours, and carry out pulse testing by the method for example 1, the separation factor recorded, MX peak width at half height and net retention volume are in table 1.
Example 3
Investigate adsorption selectivity when m-isopropyl toluene makes strippant and the Adsorption and desorption speed to extraction components.
(1) sorbent material is prepared
By NaY zeolite bead lithium ion exchanged used for example 1, exchanging liquid is the water lithium chloride solution of 0.2moL/L, and the volume ratio of lithium chloride solution used and NaY zeolite bead is 5: 1,90 DEG C, 0.1MPa, carry out lithium ion exchanged 6 hours under agitation condition.After exchange completes, filter exchange mother liquor, can't detect Cl with in deionized water wash to washings -1.Plasma emission spectrometry (ICP) measures oxide containing lithium 0.62 quality %, sodium oxide 11.54 quality % in the sample after exchanging, and sodium ion is 10% by the molar percentage of lithium ion exchanged.
(2) strippant performance is tested
By gained LiNaY zeolite pellets in 250 DEG C of nitrogen gas stream dry 2 hours, it was 3.1 quality % that 600 DEG C of roastings measure its igloss amount for 2 hours, and carry out pulse testing by the method for example 1, the separation factor recorded, MX peak width at half height and net retention volume are in table 1.
Example 4
Investigate adsorption selectivity when strippant made by m-n-propyl toluene and the Adsorption and desorption speed to extraction components.
Carry out pulse testing by the method for example 1, be made up of the m-n-propyl toluene of 30 volume % and the normal heptane of 70 volume % unlike desorption liquid, the separation factor recorded by pulse testing, MX peak width at half height and net retention volume are in table 1.
Comparative example 1
Adsorption selectivity when strippant made by toluene and the Adsorption and desorption speed to extraction components is investigated by the method for example 1, be made up of the toluene of 30 volume % and the normal heptane of 70 volume % unlike desorption liquid, the separation factor recorded by pulse testing, MX peak width at half height and net retention volume are in table 1.
Table 1

Claims (8)

1. the method for an adsorption separation of m-Xylene from C8 aronmatic, be included in the C8 aronmatic mixture containing m-xylene and adsorbent contact under liquid phase state, m-xylene is formed Adsorption Phase by adsorbent, with the m-xylene in strippant desorption Adsorption Phase, obtain the Extract comprising strippant and m-xylene, rectifying Extract obtains m-xylene, described strippant is selected from m-isopropyl toluene or m-n-propyl toluene, described sorbent material is y-type zeolite, and in its skeleton, the mol ratio of silicon oxide and aluminum oxide is 4.6 ~ 6.0.
2. in accordance with the method for claim 1, it is characterized in that described y-type zeolite is that NaY zeolite or exchangeable cation position at least 80% are occupied by sodium ion, all the other y-type zeolites occupied by the IA race metal ion except sodium ion or IIA race metal ion.
3. in accordance with the method for claim 2, it is characterized in that the described IA race metal ion except sodium is Li +, described IIA race metal ion is Sr 2+, Li +or Sr 2+exchange degree be 4 ~ 15%.
4., according to any one method described in claims 1 to 3, it is characterized in that described sorbent material is 1 ~ 6 quality % in the roasting igloss amount that 600 DEG C measure.
5., according to any one method described in claims 1 to 3, it is characterized in that the size of microcrystal of described zeolite is 0.2 ~ 1.0 micron.
6. in accordance with the method for claim 1, it is characterized in that the adsorption separation process of m-xylene and other C8 aronmatic isomer carries out having in multiple adsorbent bed simulation moving-bed device.
7. in accordance with the method for claim 6, it is characterized in that simulation moving-bed adsorbent bed absorption, purification and desorption three districts of being divided into carry out fractionation by adsorption operation.
8. in accordance with the method for claim 1, it is characterized in that the temperature of adsorbing m-xylene is 100 ~ 200 DEG C, pressure is 0.2 ~ 2.0MPa.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6137024A (en) * 1997-05-05 2000-10-24 Uop Llc Process for separating meta-xylene
CN1379007A (en) * 2001-03-29 2002-11-13 法国石油公司 Method of joint produce pare xylene and metaxylene including two stage separation
JP2007045824A (en) * 2005-08-10 2007-02-22 Inst Fr Petrole METHOD FOR SEPARATING m-XYLENE FROM AROMATIC HYDROCARBON SUPPLY MATERIAL BY LIQUID-PHASE ADSORPTION USING TETRALIN AS DESORPTION AGENT
CN102076826A (en) * 2008-06-26 2011-05-25 环球油品公司 Process and apparatus for separating para-xylene from mixture of c8 and c9 aromatic hydrocarbons
CN102167652A (en) * 2010-02-26 2011-08-31 中国石油化工股份有限公司 Adsorbent for adsorbing and separating m-xylene and preparation method of same

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7553998B2 (en) * 2006-06-21 2009-06-30 Uop Llc Energy-efficient process for para-xylene production

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6137024A (en) * 1997-05-05 2000-10-24 Uop Llc Process for separating meta-xylene
CN1379007A (en) * 2001-03-29 2002-11-13 法国石油公司 Method of joint produce pare xylene and metaxylene including two stage separation
JP2007045824A (en) * 2005-08-10 2007-02-22 Inst Fr Petrole METHOD FOR SEPARATING m-XYLENE FROM AROMATIC HYDROCARBON SUPPLY MATERIAL BY LIQUID-PHASE ADSORPTION USING TETRALIN AS DESORPTION AGENT
CN1939883A (en) * 2005-08-10 2007-04-04 法国石油公司 Process for separating meta-xylene from a feed of aromatic hydrocarbons
CN102076826A (en) * 2008-06-26 2011-05-25 环球油品公司 Process and apparatus for separating para-xylene from mixture of c8 and c9 aromatic hydrocarbons
CN102167652A (en) * 2010-02-26 2011-08-31 中国石油化工股份有限公司 Adsorbent for adsorbing and separating m-xylene and preparation method of same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
二甲苯异构体的分离技术;朱志臣等;《天津城市建设学院学报》;19970630;第3卷(第02期);71-74 *

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