WO2025145693A1 - 分离乙烯基甲苯和c9饱和芳香烃的方法和萃取剂混合物 - Google Patents

分离乙烯基甲苯和c9饱和芳香烃的方法和萃取剂混合物 Download PDF

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WO2025145693A1
WO2025145693A1 PCT/CN2024/121621 CN2024121621W WO2025145693A1 WO 2025145693 A1 WO2025145693 A1 WO 2025145693A1 CN 2024121621 W CN2024121621 W CN 2024121621W WO 2025145693 A1 WO2025145693 A1 WO 2025145693A1
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tower
extractant
glycerol
dimethylformamide
aromatic hydrocarbons
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English (en)
French (fr)
Inventor
崔婷
王宇飞
崔钟辉
王婧
过良
杨勃
常大山
陈健
刘建楠
宋潇倩
孙嵩
张全贞
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Sinopec Beijing Research Institute Of Chemical Industry Co Ltd
Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute Of Chemical Industry Co Ltd
Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Publication of WO2025145693A1 publication Critical patent/WO2025145693A1/zh
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/005—Processes comprising at least two steps in series
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C15/00—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
    • C07C15/02—Monocyclic hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C15/00—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
    • C07C15/40—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts substituted by unsaturated carbon radicals
    • C07C15/42—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts substituted by unsaturated carbon radicals monocyclic
    • C07C15/44—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts substituted by unsaturated carbon radicals monocyclic the hydrocarbon substituent containing a carbon-to-carbon double bond
    • C07C15/46—Styrene; Ring-alkylated styrenes
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/04—Purification; Separation; Use of additives by distillation
    • C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids

Definitions

  • the invention relates to aromatic hydrocarbon separation, in particular to a method for separating vinyl toluene and C9 saturated aromatic hydrocarbons from light cracked C9 aromatic hydrocarbons and an extractant mixture.
  • Cracking C9 is one of the by-products of petroleum cracking, containing a large amount of C9 aromatics (also known as cracked C9 aromatics), such as indene, vinyl toluene, propylbenzene, methyl ethyl benzene and trimethylbenzene.
  • C9 aromatics also known as cracked C9 aromatics
  • cracked C9 aromatics are used directly without treatment, for example, as a gasoline blending component.
  • it is used to produce petroleum resins with very low added value, but most of the components contained therein are not fully utilized. Direct use of cracked C9 aromatics leads to low resource utilization and economic added value.
  • CN 107502386 A introduces a method for obtaining mixed aromatics by hydrogenation separation of cracked C9 fractions.
  • the method includes: removing heavy components such as colloids in the cracked C9 fraction; low-temperature liquid phase hydrogenation to remove easily polymerizable components such as diolefins; high-temperature gas phase hydrogenation to remove monoolefins, sulfur and nitrogen; and distillation separation to obtain mixed aromatics with low non-aromatic content.
  • the hydrogenation reaction of this process also removes active monomers such as styrene in the cracked C9 fraction, which results in low resource utilization, high cost and low economic added value.
  • the boiling points of various components in cracked C9 aromatics are close.
  • the boiling point of 2-methylstyrene is about 169°C
  • the boiling point of 3-methylstyrene is about 170°C
  • the boiling point of 4-methylstyrene is about 171°C.
  • the alkyl-substituted benzenes with nine carbon atoms C9 saturated aromatic hydrocarbons
  • the boiling point of 2-ethyltoluene is about 165°C
  • the boiling point of 4-ethyltoluene is about 162°C
  • the boiling point of mesitylene is about 167°C
  • the boiling point of para-trimethylbenzene is about 168°C. Since vinyltoluene and C9 saturated aromatic hydrocarbons have close boiling points and similar structures, it is difficult to separate them from each other using ordinary distillation methods.
  • Extractive distillation has been proposed in the art to separate substances. However, there is no report on the use of extractive distillation to separate vinyl toluene and C9 saturated aromatic hydrocarbons with a boiling point close to that of vinyl toluene.
  • the present invention provides a method for separating vinyl toluene and C9 saturated aromatic hydrocarbons represented by C9H12 , comprising the following steps:
  • the present invention provides an extractant mixture for separating vinyltoluene and C9 saturated aromatic hydrocarbons represented by C9H12 by extractive distillation, wherein the extractant mixture comprises N,N-dimethylformamide and glycerol.
  • the inventors of the present invention unexpectedly discovered that vinyltoluene and C9 saturated aromatic hydrocarbons can be effectively separated by extractive distillation using an extractant mixture comprising N,N-dimethylformamide (DMF) and glycerol (GLY).
  • the present invention was completed based on the above discovery.
  • the method of the present invention can continuously separate vinyltoluene and C9 saturated aromatic hydrocarbons from light cracked carbon nine aromatic hydrocarbons, achieving high yield and purity. For example, the purity of vinyltoluene can reach greater than or equal to 90%, and the yield can reach greater than or equal to 85%; the purity of C9 saturated aromatic hydrocarbons can reach greater than or equal to 65%.
  • FIG. 1 is a process flow diagram of one embodiment of the method of the present invention.
  • any specific numerical value disclosed herein is not limited to the exact value of the numerical value, but should be understood to also cover values close to the exact value, such as all possible numerical values within the range of ⁇ 5% of the exact value.
  • the endpoint values of the range, the endpoint values and the specific point values in the range, and the specific point values can be arbitrarily combined to obtain one or more new numerical ranges, and these new numerical ranges should also be regarded as specifically disclosed herein.
  • the removal of heavy components from the cracked C9 aromatics can be carried out by various methods known in the art. For example, two towers are used to treat the cracked C9 aromatics, wherein the dicyclopentadiene contained in the cracked C9 aromatics is depolymerized into cyclopentadiene in the first tower, and the cyclopentadiene is removed, and then the removed heavy components are removed. The logistics after the dicyclopentadiene is removed is passed into a second tower to remove other heavy components to obtain the light cracked C9 aromatics.
  • the extractant mixture used in the present invention comprises N,N-dimethylformamide and glycerol.
  • the extractant mixture used in the present invention consists of N,N-dimethylformamide and glycerol.
  • the extractant mixture comprises N,N-dimethylformamide, glycerol and an auxiliary extractant, wherein the auxiliary extractant is selected from cyclopentane sulfone, dimethyl sulfoxide, and phenol.
  • the amount of the auxiliary extractant is selected so as not to affect the extraction distillation.
  • the extractant mixture comprises 0-50% by weight, preferably 0-20% by weight, and more preferably 0-10% by weight of the auxiliary extractant.
  • the bottom fraction contains vinyltoluene, glycerol and the auxiliary extractant. Accordingly, in step (3), the bottom fraction can be refined in a vinyltoluene refining tower to obtain a stream rich in vinyltoluene at the top of the tower, and a stream containing glycerol and the auxiliary extractant at the bottom of the tower.
  • the extractant mixture enters from the upper part of the extractive distillation tower, and the light cracked carbon nine aromatics enter from the middle part of the extractive distillation tower.
  • Such an arrangement can achieve better countercurrent contact between the extractant mixture and the distillate in the extractive distillation tower.
  • the feed temperature of the extractant mixture is 10-30°C, and the extractant mixture can be fed at room temperature (25°C).
  • the extractant mixture and the light cracked C9 aromatics are introduced into the extractive distillation tower at a mass flow rate ratio of 0.1-1.5, preferably 0.1-0.6, more preferably 0.2-0.4.
  • the extractive distillation tower is provided with a light cracked C9 aromatic hydrocarbon feed pipeline, an extractant mixture feed pipeline, an extractive distillation tower overhead fraction discharge pipeline, and an extractive distillation tower bottom fraction discharge pipeline; wherein the extractive distillation tower is connected to the C9 saturated aromatic hydrocarbon refining tower through the extractive distillation tower overhead fraction discharge pipeline, and is connected to the vinyltoluene refining tower through the extractive distillation tower bottom fraction discharge pipeline.
  • step (2) the N,N-dimethylformamide obtained at the top of the tower can be returned to the extractive distillation tower for recycling.
  • step (3) the glycerol and optional auxiliary extractant obtained at the bottom of the tower are It can be returned to the extraction distillation tower for recycling.
  • the C9 saturated aromatic hydrocarbon refining tower is provided with an overhead fraction discharge pipeline at the top and a bottom fraction discharge pipeline at the bottom; wherein the overhead fraction discharge pipeline is connected to the extractant mixture feed pipeline.
  • the vinyltoluene refining tower is provided with an overhead fraction discharge pipeline at the top and a bottom fraction discharge pipeline at the bottom; wherein the bottom fraction discharge pipeline of the vinyltoluene refining tower is connected to the extractant mixture feed pipeline.
  • the operating conditions of the extractive distillation tower include: the number of theoretical plates is 50-90, the operating pressure is 5-20 kPa, the bottom temperature is 250-330° C., and the reflux ratio is 15-25.
  • the present invention provides an extractant mixture for separating vinyl toluene and C9 saturated aromatic hydrocarbons represented by C9H12 by extractive distillation, wherein the extractant mixture comprises N,N-dimethylformamide and glycerol, and the mass ratio of N,N-dimethylformamide to glycerol is 0.05-0.5:1, preferably 0.06-0.12:1.
  • the extractant mixture used in the present invention consists of N,N-dimethylformamide and glycerol.
  • the present invention may be embodied in the following embodiments:
  • step (1) passing the mixed aromatics-rich fraction obtained from the top of the tower in step (1) into a mixed aromatics
  • the hydrocarbon refining tower is used for refining, and the extractant obtained at the top of the tower is returned to the extraction distillation tower for recycling, and high-quality mixed aromatics are obtained at the bottom of the tower;
  • step (3) The 2-methylstyrene-rich fraction obtained at the bottom of the tower in step (1) is passed into a 2-methylstyrene refining tower for refining, and high-purity 2-methylstyrene is obtained at the top of the tower.
  • the extractant obtained at the bottom of the tower is returned to the extractive distillation tower for recycling.
  • the method comprises: the number of theoretical plates is 50-90, the operating pressure is normal pressure, the reflux ratio is 5-20, and the bottom temperature is 360-380°C.
  • the light cracked carbon nine aromatics used in the following examples are composed of the following components (by weight): 5.6% allylbenzene, 3.7% n-propylbenzene, 10.6% 2-ethyltoluene, 2.3% 3-ethyltoluene, 3.7% 4-ethyltoluene, 7.2% 1,3,5-trimethylbenzene, 2.8% 1,2,4-trimethylbenzene, 1.8% 1,2,3-trimethylbenzene, 6.6% isopropylbenzene, 55.1% 2-methylstyrene, and 0.6% dicyclopentadiene.
  • the tower bottom fraction of the extractive distillation tower 1 is passed to the vinyl toluene refining tower 3 for refining, a stream d rich in vinyl toluene is obtained at the top of the tower, and GLY and an optional auxiliary extractant are obtained at the bottom of the tower, wherein the GLY and the optional auxiliary extractant obtained at the bottom of the tower are returned to the extractive distillation tower 1 for recycling.
  • the quality of the vinyl toluene-rich logistics d and the vinyl toluene therein, the C9 saturated aromatic hydrocarbon-rich logistics c and the C9 saturated aromatic hydrocarbons therein obtained in the embodiments and comparative examples was tested, and the corresponding purity and yield were calculated.
  • the C9 saturated aromatic hydrocarbons are n-propylbenzene, 2-ethyltoluene, 3-ethyltoluene, 4-ethyltoluene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene, 1,2,3-trimethylbenzene and isopropylbenzene, and the vinyl toluene is 2-methylstyrene.
  • Purity of vinyl toluene mass of vinyl toluene/mass of stream d rich in vinyl toluene ⁇ 100%;
  • C9 saturated aromatic hydrocarbons mass of C9 saturated aromatic hydrocarbons/mass of stream c rich in C9 saturated aromatic hydrocarbons ⁇ 100%;
  • the yield of vinyl toluene the mass of vinyl toluene / the ethylene content of light cracked carbon nine aromatics The mass of methylbenzene ⁇ 100%;
  • the mass of vinyl toluene in the light cracked carbon nine aromatics is the product of the content of vinyl toluene (55.1%) and the input amount of the light cracked carbon nine aromatics;
  • the mass of mixed aromatics in light cracked C9 aromatics is the product of the content of C9 saturated aromatics (3.7% + 10.6% + 2.3% + 3.7% + 7.2% + 2.8% + 1.8% + 6.6%) and the input amount of light cracked C9 aromatics.
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 15, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 15, and a bottom temperature of 377° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and GLY is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 70, a reflux ratio of 15, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 70, a reflux ratio of 10, and a bottom temperature of 377° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and GLY is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 15, and a bottom temperature of 259° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is introduced into a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operating at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, a bottom temperature of 258° C., DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyl toluene refining tower 3 for refining, wherein the operating conditions of the vinyl toluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 377° C.
  • the operating conditions of the vinyl toluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 377° C.
  • a stream d rich in vinyl toluene is obtained at the top of the tower, and GLY is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 70, a reflux ratio of 15, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 15, and a bottom temperature of 377° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and GLY is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is introduced into a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operating at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, a bottom temperature of 258° C., DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 372° C.
  • the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 372° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and GLY is obtained at the bottom of the tower.
  • step (1) The top fraction of step (1) is introduced into a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, which is optionally returned to the extractive distillation tower 1 for recycling, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C.
  • DMF is obtained at the top of the tower, which is optionally returned to the extractive distillation tower 1 for recycling, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is introduced into a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 374° C.
  • a vinyltoluene-rich stream d is obtained at the top of the tower, and GLY is obtained at the bottom of the tower, which can be optionally returned to the extractive distillation tower for recycling.
  • Light cracked carbon nine aromatic hydrocarbons a are fed from the middle of an extractive distillation tower 1, and an extractant mixture b (a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and dimethyl sulfoxide as an auxiliary extractant, the mass ratio of the three being 1:9:90) is fed from the upper part of the extractive distillation tower 1 at room temperature to perform extractive distillation to obtain a tower top fraction and a tower bottom fraction, wherein the mass flow ratio of the extractant mixture b to the light cracked carbon nine aromatic hydrocarbons a is 0.3, and the extractant mixture b is 0.5:1.
  • the operating conditions of the distillation tower 1 include: the theoretical plate number is 60, the operating pressure is 10 kPa, the bottom temperature is 277° C., and the reflux ratio is 20.
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 290° C.
  • the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 290° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and a mixed liquid of GLY and dimethyl sulfoxide is obtained at the bottom of the tower.
  • Light cracked carbon nine aromatic hydrocarbons a are fed from the middle of an extractive distillation tower 1, and a mixed solution of an extractant mixture b (a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and cyclopentane sulfone, the mass ratio of the three being 1:9:10) is fed from the upper part of the extractive distillation tower 1 at room temperature, and extractive distillation is performed to obtain a tower top fraction and a tower bottom fraction, wherein the mass flow ratio of the extractant mixture b to the light cracked carbon nine aromatic hydrocarbons a is 0.3, and the operating conditions of the extractive distillation tower 1 include: a theoretical plate number of 60, an operating pressure of 10 kPa, a bottom temperature of 280°C, and a reflux ratio of 20.
  • an extractant mixture b a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and cyclopentane sulfone, the
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyl toluene refining tower 3 for refining, wherein the operating conditions of the vinyl toluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 377° C.
  • the operating conditions of the vinyl toluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 377° C.
  • a stream d rich in vinyl toluene is obtained at the top of the tower, and a mixed liquid of GLY and cyclopentane is obtained at the bottom of the tower.
  • Light cracked carbon nine aromatic hydrocarbons a are fed from the middle of an extractive distillation tower 1, and an extractant mixture b (a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and phenol, the mass ratio of the three being 1:9:10) is fed from the upper part of the extractive distillation tower 1 at room temperature to perform extractive distillation to obtain a tower top fraction and a tower bottom fraction, wherein the mass flow rate ratio of the extractant mixture b to the light cracked carbon nine aromatic hydrocarbons a is 0.3, and the operating conditions of the extractive distillation tower 1 include: a theoretical plate number of 60, an operating pressure of 10 kPa, a bottom temperature of 276°C, and a reflux ratio of 20.
  • an extractant mixture b a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and phenol, the mass ratio of the three being 1:9:10
  • the operating conditions of the extractive distillation tower 1
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) The bottom fraction of step (1) is passed to a vinyltoluene refining tower 3 for refining, wherein the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 300° C.
  • the operating conditions of the vinyltoluene refining tower 3 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 300° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and a mixed liquid of GLY and phenol is obtained at the bottom of the tower.
  • Light cracked carbon nine aromatic hydrocarbons a are fed from the middle of an extractive distillation tower 1, and a mixed solution of an extractant mixture b (a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and dimethyl sulfoxide, the mass ratio of the three being 1:9:10) is fed from the upper part of the extractive distillation tower 1 at room temperature, and extractive distillation is performed to obtain a tower top fraction and a tower bottom fraction, wherein the mass flow rate ratio of the extractant mixture b to the light cracked carbon nine aromatic hydrocarbons a is 0.3, and the operating conditions of the extractive distillation tower 1 include: a theoretical plate number of 60, an operating pressure of 10 kPa, a bottom temperature of 276°C, and a reflux ratio of 20.
  • an extractant mixture b a mixed solution of N,N-dimethylformamide (DMF), glycerol (GLY) and dimethyl sulfoxide, the mass ratio of the three being 1
  • step (1) The top fraction of step (1) is passed to a C9 saturated aromatic hydrocarbon refining tower 2 for refining, wherein the operating conditions of the C9 saturated aromatic hydrocarbon refining tower 2 include: operation at normal pressure, a theoretical plate number of 60, a reflux ratio of 20, and a bottom temperature of 258° C. DMF is obtained at the top of the tower, and a stream c rich in C9 saturated aromatic hydrocarbons is obtained at the bottom of the tower.
  • step (1) the bottom fraction of step (1) is passed into a vinyltoluene refining tower 3 for refining
  • the operating conditions of the vinyltoluene refining tower 3 include: operating at normal pressure, a theoretical plate number of 60, a reflux ratio of 10, and a bottom temperature of 310° C.
  • a stream d rich in vinyltoluene is obtained at the top of the tower, and a mixed liquid of GLY and dimethyl sulfoxide is obtained at the bottom of the tower.
  • Example 6 was repeated, except that only DMF was used as the extractant.
  • Example 6 was repeated, except that only GLY was used as the extractant.
  • Example 6 was repeated, except that the extractant mixture was a mixed solution of N,N-dimethylformamide (DMF) and glycerol (GLY), wherein the mass ratio of the two was 0.67:1.
  • DMF N,N-dimethylformamide
  • GLY glycerol
  • the method of the present invention effectively separates vinyl toluene and C9 saturated aromatic hydrocarbons, and obtains improved purity and yield.

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Abstract

本发明涉及分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法和萃取剂混合物。本发明方法包括步骤：(1)提供含有乙烯基甲苯和C9饱和芳香烃的物流；(2)将所述物流与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。本发明方法可以用于从轻质裂解碳九芳烃中分离乙烯基甲苯和C9饱和芳香烃，实现高收率和高纯度。

Description

分离乙烯基甲苯和C9饱和芳香烃的方法和萃取剂混合物 技术领域
本发明涉及芳烃分离，具体地涉及一种从轻质裂解碳九芳烃中分离乙烯基甲苯和C9饱和芳香烃的方法和萃取剂混合物。
背景技术
裂解碳九是石油裂解的副产物之一，含有大量的碳九芳烃(又称为裂解碳九芳烃)，如茚、乙烯基甲苯、丙苯、甲乙苯和三甲苯等。目前，在大多数情况下，裂解碳九芳烃未经处理而直接使用，例如被作为汽油调和组分。也有用来生产附加值很低的石油树脂的情况，但其中所含的大部分组分得不到充分利用。直接利用裂解碳九芳烃导致低资源利用率和经济附加值。
本领域中已经提出多种方法，以从裂解碳九或裂解碳九芳烃中分离其中的某个或某些组分。例如，CN 107502386 A介绍了一种裂解碳九馏分经加氢分离获取混合芳烃的方法。所述方法包括：除去裂解碳九馏分中的胶质等重组分；低温液相加氢，以去除双烯烃等易聚合组分；高温气相加氢，以脱除单烯烃、硫和氮；精馏分离，以获得非芳含量较低的混合芳烃。该工艺的加氢反应也去除了裂解碳九馏分中的苯乙烯等活性单体，这使得资源利用率低，成本高，经济附加值低。
乙烯基甲苯，如2-甲基苯乙烯，是重要的有机合成单体，特别是用于医药研发。本领域中通过乙醇和甲苯反应来合成乙烯基甲苯。该方法存在众多缺点，如原料价格昂贵、反应效率低、能耗大、设备投入高等。裂解碳九芳烃中含有乙烯基甲苯。因此，从裂解碳九芳烃中高效分离乙烯基甲苯将是上述合成的有利替代。
裂解碳九芳烃中的多种组分的沸点接近。其中，2-甲基苯乙烯的沸点为约169℃，3-甲基苯乙烯的沸点为约170℃，4-甲基苯乙烯的沸点为约171℃。具有九个碳原子的烷基取代的苯(C9饱和芳香烃)中，2-乙基甲苯的沸点为约165℃、4-乙基甲苯的沸点为约162℃、均三甲苯的沸点为约167℃、偏三甲苯的沸点为约168℃。由于乙烯基甲苯与C9饱和芳香烃的沸点接近并且结构相似，因此采用普通的精馏方法难以将它们彼此分开。
本领域中已经提出采用萃取精馏进行物质的分离。但是，还没有使用萃取精馏分离乙烯基甲苯和与其沸点接近的C9饱和芳香烃的报道。
发明内容
本发明的目的是为了克服现有技术难以分离乙烯基甲苯和C9饱和芳香烃的问题。本发明提供一种从含有乙烯基甲苯和C9饱和芳香烃的物流中分离乙烯基甲苯和C9饱和芳香烃的方法，其使用包含N,N-二甲基甲酰胺和甘油的萃取剂混合物通过萃取精馏进行所述分离。本发明方法可以用于从(轻质)裂解碳九芳烃中分离乙烯基甲苯和C9饱和芳香烃，实现高收率和高纯度。
在一个方面，本发明提供一种分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
(1)提供含有乙烯基甲苯和C9饱和芳香烃的物流；
(2)将所述物流与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油的混合溶液，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
在另一个方面，本发明提供一种从轻质裂解碳九芳烃中分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
(1)将轻质裂解碳九芳烃与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
在另外一个方面，本发明提供一种用于通过萃取精馏来分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的萃取剂混合物，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油。
本发明的发明人意外发现，以包含N,N-二甲基甲酰胺(DMF)和甘油(GLY)的萃取剂混合物通过萃取精馏可以有效分离乙烯基甲苯和C9饱和芳香烃。基于上述发现完成了本发明。本发明方法可以连续地从轻质裂解碳九芳烃中分离乙烯基甲苯和C9饱和芳香烃，实现高的收率和纯度。例如，乙烯基甲苯的纯度可达到大于等于90％，收率可达到大于等于85％；C9饱和芳香烃的纯度可达到大于等于65％。
附图说明
图1是本发明方法的一个实施方案的工艺流程图。
附图标记说明
1萃取精馏塔；2 C9饱和芳香烃精制塔；3乙烯基甲苯精制塔；
a轻质裂解碳九芳烃；b萃取剂混合物；c富含C9饱和芳香烃的物流；d富含乙烯基甲苯的物流。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
在本文中所披露的任何具体数值(包括数值范围的端点)都不限于该数值的精确值，而应当理解为还涵盖了接近该精确值的值，例如在该精确值±5％范围内的所有可能的数值。并且，对于所披露的数值范围而言，在该范围的端点值之间、端点值与范围内的具体点值之间，以及各具体点值之间可以任意组合而得到一个或多个新的数值范围，这些新的数值范围也应被视为在本文中具体公开。
除了在实施例外，在本文中，参数的所有数值都应理解为在所有情况下均由术语“约”修饰，无论“约”是否实际上出现在该数值之前。
除非另有其他明确表示，否则在整个说明书和权利要求书中，术语“包括”或其变换如“包含”或“含有”等将被理解为包括所陈述的元件或组成部分，而并未排除其他元件或其他组成部分。此外，术语“包括”或其变换如“包含”或“含有”等也可以排除其他元件或其他组成部分，即“由…组成”或“基本上由…组成”的情况。
在一个方面，本发明提供一种分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
(1)提供含有乙烯基甲苯和C9饱和芳香烃的物流；
(2)将所述物流与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
在本文中，“乙烯基甲苯”选自1-甲基苯乙烯、2-甲基苯乙烯、3-甲基苯乙烯和其混合物。乙烯基甲苯的沸点取决于1-甲基苯乙烯、2-甲基苯乙烯和3-甲基苯乙烯各自的量，其通常为169-171℃。在一个变型中，乙烯基甲苯为2-甲基苯乙烯。
在本文中，“C9H12表示的C9饱和芳香烃”指的是具有九个碳原子并且取代基均为烷基的苯环，其可以包括：丙苯、甲乙苯和三甲苯中的一种或多种。所述C9饱和芳香烃中的某些成分具有与所述乙烯基甲苯相同或相近的沸点，例如2-乙基甲苯(沸点为约165℃)、4-乙基甲苯(沸点为约162℃)、均三甲苯(沸点为约167℃)、偏三甲苯(沸点为约168℃)、等等。
在一个变型中，含有乙烯基甲苯和C9饱和芳香烃的物流由乙烯基甲苯和C9饱和芳香烃组成，或基本上由乙烯基甲苯和C9饱和芳香烃组成。在后一种情况中，乙烯基甲苯和C9饱和芳香烃占物流的大于等于85重量％，优选大于等于90重量％，更优选大于等于95重量％，最优选大于等于98重量％。
本发明所用萃取剂混合物包含N,N-二甲基甲酰胺和甘油。在一种情况下，本发明所用萃取剂混合物由N,N-二甲基甲酰胺和甘油构成。在另一种情况下，所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚。选择辅助萃取剂的用量以便不影响萃取精馏的进行。在一个优选方案中所述萃取剂混合物包含0-50重量％，优选0-20重量％，更优选0-10重量％的辅助萃取剂。N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80-100重量％，更优选90-100重量％。优选地，在上述两种情况下，所述N,N-二甲基甲酰胺和所述甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。本发明发明人意外发现，控制N,N-二甲基甲酰胺和甘油的质量比在上述范围内时，有助于获得更好的分离效果。
根据本发明一种优选实施方式，所述塔顶馏分和塔底馏分可以分别进行精制，以获得乙烯基甲苯和C9饱和芳香烃。例如，含有C9饱和芳香烃和N,N-二甲基甲酰胺的所述塔顶馏分可以在C9饱和芳香烃精制塔中进行精制，在塔顶得到N,N-二甲基甲酰胺，并在塔底得到富含C9饱和芳香烃的物流。含有乙烯基甲苯和甘油的所述塔底馏分可以在 乙烯基甲苯精制塔中进行精制，在塔顶得到富含乙烯基甲苯的物流，并在塔底得到甘油。在萃取剂混合物含有辅助萃取剂的情况下，所述塔底馏分含有乙烯基甲苯、甘油和辅助萃取剂。相应地，所述塔底馏分可以在乙烯基甲苯精制塔中进行精制，在塔顶得到富含乙烯基甲苯的物流，并在塔底得到含有甘油和辅助萃取剂的物流。
本发明方法可以有效分离乙烯基甲苯和C9H12表示的C9饱和芳香烃，使其特别适用于从轻质裂解碳九芳烃中分离乙烯基甲苯和C9H12表示的C9饱和芳香烃。相应地，本发明提供一种从轻质裂解碳九芳烃中分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
(1)将轻质裂解碳九芳烃与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
在一个优选方案中，本发明方法进一步包括以下步骤：
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔进行精制，在塔顶得到N,N-二甲基甲酰胺，并在塔底得到富含C9饱和芳香烃的物流；
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔进行精制，在塔顶得到富含乙烯基甲苯的物流，并在塔底得到甘油。
在本文中，术语“轻质裂解碳九芳烃”为裂解碳九芳烃脱除重组分后得到的物流。术语“裂解碳九芳烃”指的是石油裂解副产品中的一种，其含有具有九个碳原子的芳烃馏分。所述芳烃馏分包括茚、乙烯基甲苯、丙苯、甲乙苯和三甲苯等，其分别具有不同沸点。裂解碳九芳烃中也可能存在具有超过九个碳原子的馏分，例如双环戊二烯。通常，将沸点大于等于茚的沸点(约182℃)的组分称为裂解碳九芳烃的重组分。裂解碳九芳烃进行脱除重组分后得到所述轻质裂解碳九芳烃，其可以包含乙烯基甲苯、丙苯、甲乙苯和三甲苯。所述轻质裂解碳九芳烃可以含有一些杂质，例如残留的重组分。显然，所述轻质裂解碳九芳烃也是一种含有乙烯基甲苯和C9饱和芳香烃的物流。
从裂解碳九芳烃脱除重组分可以采用本领域公知的各种方法进行。例如，采用两个塔处理裂解碳九芳烃，其中在第一个塔中将裂解碳九芳烃中含有的双环戊二烯解聚为环戊二烯，并将环戊二烯脱除，然后将脱 除双环戊二烯后的物流通入第二个塔脱除其它重组分，得到所述轻质裂解碳九芳烃。
本发明所用萃取剂混合物包含N,N-二甲基甲酰胺和甘油。在一种情况下，本发明所用萃取剂混合物由N,N-二甲基甲酰胺和甘油构成。在另一种情况下，所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚。选择辅助萃取剂的用量以便不影响萃取精馏的进行。在一个优选方案中所述萃取剂混合物包含0-50重量％，优选0-20重量％，更优选0-10重量％的辅助萃取剂。N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80-100重量％，更优选90-100重量％。优选地，在两种情况下，N,N-二甲基甲酰胺和甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。本发明发明人意外发现，控制N,N-二甲基甲酰胺和甘油的质量比在上述范围内时，有助于获得更好的分离效果。
在萃取剂混合物含有辅助萃取剂的情况下，所述塔底馏分含有乙烯基甲苯、甘油和辅助萃取剂。相应地，在步骤(3)中，所述塔底馏分可以在乙烯基甲苯精制塔中进行精制，在塔顶得到富含乙烯基甲苯的物流，并在塔底得到含有甘油和辅助萃取剂的物流。
根据本发明一种优选实施方式，所述萃取剂混合物从萃取精馏塔的上部进入，所述轻质裂解碳九芳烃从萃取精馏塔的中部进入。这样的设置可以使萃取剂混合物与馏分在萃取精馏塔中实现更好的逆流接触。
根据本发明一种优选实施方式，所述萃取剂混合物的进料温度为10-30℃，可在常温(25℃)下进料。
根据本发明一种优选实施方式，所述萃取剂混合物与轻质裂解碳九芳烃以质量流量之比为0.1-1.5，优选为0.1-0.6，更优选为0.2-0.4通入萃取精馏塔。
根据本发明一种优选实施方式，所述萃取精馏塔设置有轻质裂解碳九芳烃进料管线、萃取剂混合物进料管线、萃取精馏塔塔顶馏分出料管线、萃取精馏塔塔底馏分出料管线；其中所述萃取精馏塔通过所述萃取精馏塔塔顶馏分出料管线与所述C9饱和芳香烃精制塔连接、通过所述萃取精馏塔塔底馏分出料管线与所述乙烯基甲苯精制塔连接。
步骤(2)中，在塔顶得到的N,N-二甲基甲酰胺可以被返回萃取精馏塔循环使用。步骤(3)中，在塔底得到的甘油和任选的辅助萃取剂 可以被返回萃取精馏塔循环使用。
所述C9饱和芳香烃精制塔塔顶设置有塔顶馏分出料管线、塔底设置有塔底馏分出料管线；其中所述塔顶馏分出料管线与所述萃取剂混合物进料管线连接。
所述乙烯基甲苯精制塔塔顶设置塔顶馏分出料管线、塔底设置有塔底馏分出料管线；其中所述乙烯基甲苯精制塔的塔底馏分出料管线与所述萃取剂混合物进料管线连接。
优选地，所述萃取精馏塔的操作条件包括：理论塔板数为50-90块，操作压力为5-20kPa，塔釜温度为250-330℃，回流比为15-25。
优选地，所述C9饱和芳香烃精制塔的操作条件包括：理论塔板数为40-80块，操作压力为常压，回流比为10-25，塔釜温度为250-265℃。
优选地，所述乙烯基甲苯精制塔的操作条件包括：理论塔板数为50-90块，操作压力为常压，回流比为5-20，塔釜温度为280-380℃。
另一方面，本发明提供一种用于通过萃取精馏来分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的萃取剂混合物，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，N,N-二甲基甲酰胺和甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。在一种情况下，本发明所用萃取剂混合物由N,N-二甲基甲酰胺和甘油构成。在另一种情况下，所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚。选择辅助萃取剂的用量以便不影响萃取精馏的进行。在一个优选方案中所述萃取剂混合物包含0-50重量％，优选0-20重量％，更优选0-10重量％的辅助萃取剂。N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80-100重量％，更优选90-100重量％。
例如，本发明可以体现在以下方案：
1、一种萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，包括以下步骤：
(1)将原料轻质裂解碳九芳烃与萃取剂通入萃取精馏塔进行萃取精馏，塔顶得到富含混合芳烃的馏分，塔底得到富含2-甲基苯乙烯的馏分；所述萃取剂为N,N-二甲基甲酰胺和甘油的复合溶液；
(2)将步骤(1)中塔顶得到的富含混合芳烃的馏分通入到混合芳 烃精制塔进行精制，塔顶得到萃取剂返回萃取精馏塔循环使用，塔底得到高质量的混合芳烃；
(3)将步骤(1)中塔底得到的富含2-甲基苯乙烯的馏分通入到2-甲基苯乙烯精制塔进行精制，塔顶得到高纯的2-甲基苯乙烯，塔底得到萃取剂返回萃取精馏塔循环使用。
2、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述轻质裂解碳九芳烃为裂解碳九芳烃脱除双环戊二烯和脱除重组分后得到的轻质裂解碳九芳烃。
3、方案2所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述重组分为具有10个以上碳原子的组分。
4、方案2所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述轻质裂解碳九芳烃为C6～C9的芳烃。
5、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述N,N-二甲基甲酰胺和所述甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。
6、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述萃取剂从萃取精馏塔的精馏段进入，所述萃取剂的进料温度为10-30℃。
7、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述萃取剂与原料的质量流量之比为0.1-1.5，优选为0.1-0.6，更优选为0.2-0.4。
8、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述萃取精馏塔的操作条件包括：理论塔板数为50-90块，操作压力为5-20kPa，塔釜温度为300-330℃，回流比为15-25。
9、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述混合芳烃精制塔的操作条件包括：理论塔板数为40-80块，操作压力为常压，回流比为10-25，塔釜温度为250-265℃。
10、方案1所述的萃取精馏分离轻质裂解碳九芳烃中的2-甲基苯乙烯和混合芳烃的方法，其中，所述2-甲基苯乙烯精制塔的操作条件 包括：理论塔板数为50-90块，操作压力为常压，回流比为5-20，塔釜温度为360-380℃。
实施例
下面结合实施例对本发明作进一步说明，但本发明的范围并不局限于这些实施例。
以下实施例中所采用的轻质裂解碳九芳烃由以下的组分(重量计)组成：烯丙苯5.6％、正丙苯3.7％、2-乙基甲苯10.6％、3-乙基甲苯2.3％、4-乙基甲苯3.7％、1,3,5-三甲基苯7.2％、1,2,4-三甲基苯2.8％、1,2,3-三甲基苯1.8％、异丙苯6.6％、2-甲基苯乙烯55.1％、双环戊二烯0.6％。
以下实施例均采用如图1所示的工艺流程。具体地说，轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分。萃取精馏塔1的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c，其中在塔顶得到的DMF被返回萃取精馏塔1循环使用。萃取精馏塔1的塔底馏分通入到乙烯基甲苯精制塔3进行精制，在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY和任选的辅助萃取剂，其中在塔底得到的GLY和任选的辅助萃取剂被返回萃取精馏塔1循环使用。
测试方法
对实施例和对比例中获得的富含乙烯基甲苯的物流d及其中的乙烯基甲苯、富含C9饱和芳香烃的物流c及其中的C9饱和芳香烃的质量进行测试，并计算相应的纯度和收率。对于所用的轻质裂解碳九芳烃，所述C9饱和芳香烃为正丙苯、2-乙基甲苯、3-乙基甲苯、4-乙基甲苯、1,3,5-三甲基苯、1,2,4-三甲基苯、1,2,3-三甲基苯和异丙苯，并且所述乙烯基甲苯为2-甲基苯乙烯。
纯度和收率分别采用如下公式进行计算：
乙烯基甲苯的纯度＝乙烯基甲苯的质量/富含乙烯基甲苯的物流d的质量×100％；
C9饱和芳香烃的纯度＝C9饱和芳香烃的质量/富含C9饱和芳香烃的物流c的质量×100％；
乙烯基甲苯的收率＝乙烯基甲苯的质量/轻质裂解碳九芳烃中乙烯 基甲苯的质量×100％；
C9饱和芳香烃的收率＝C9饱和芳香烃的质量/轻质裂解碳九芳烃中C9饱和芳香烃的质量×100％，
其中，轻质裂解碳九芳烃中乙烯基甲苯的质量为乙烯基甲苯的含量(55.1％)与轻质裂解碳九芳烃输入量的乘积；
轻质裂解碳九芳烃中混合芳烃的质量为C9饱和芳香烃的含量(3.7％+10.6％+2.3％+3.7％+7.2％+2.8％+1.8％+6.6％)与轻质裂解碳九芳烃输入量的乘积。
实施例1
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.1：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.5，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为15kPa、塔釜温度为320℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为15，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为15，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例2
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.15：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a 的质量流量之比为0.5，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为310℃、回流比为15。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为70、回流比为15，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为70、回流比为10，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例3
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.12：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.5，萃取精馏塔1的操作条件包括：理论塔板数为70、操作压力为10kPa、塔釜温度为330℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为15，塔釜温度为259℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例4
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.35：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为80、操作压力为10kPa、塔釜温度为300℃、回流比为15。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃，在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为15，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例5
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.08：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为320℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃，在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例6
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.24：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为20kPa、塔釜温度为310℃、回流比为15。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为70、回流比为15，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为15，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例7
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.43：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为295℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃，在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为372℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例8
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，二者质量比为0.06：1)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为301℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃，在塔顶得到DMF，其任选被返回萃取精馏塔1循环使用，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为374℃。在塔顶得到富乙烯基甲苯的物流d，并在塔底得到GLY，其任选被返回萃取精馏塔循环使用。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例9
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)、甘油(GLY)以及作为辅助萃取剂的二甲基亚砜的混合溶液，三者质量比为1：9：90)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精 馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为277℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为290℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY与二甲基亚砜的混合液。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例10
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)、甘油(GLY)以及环丁砜)的混合溶液，三者质量比为1：9：10)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为280℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为377℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY与环丁砜的混合液。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例11
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)、甘油(GLY)以及苯酚)的混合溶液，三者质量比为1：9：10)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为276℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制，其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为300℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY与苯酚的混合液。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
实施例12
(1)将轻质裂解碳九芳烃a从萃取精馏塔1中部进料，萃取剂混合物b(N,N-二甲基甲酰胺(DMF)、甘油(GLY)以及二甲基亚砜)的混合溶液，三者质量比为1：9：10)从萃取精馏塔1的上部在室温进料，进行萃取精馏，得到塔顶馏分和塔底馏分，其中萃取剂混合物b与轻质裂解碳九芳烃a的质量流量之比为0.3，萃取精馏塔1的操作条件包括：理论塔板数为60、操作压力为10kPa、塔釜温度为276℃、回流比为20。
(2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔2进行精制，其中C9饱和芳香烃精制塔2的操作条件包括：在常压下操作、理论塔板数为60、回流比为20，塔釜温度为258℃。在塔顶得到DMF，并在塔底得到富含C9饱和芳香烃的物流c。
(3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔3进行精制， 其中乙烯基甲苯精制塔3的操作条件包括：在常压下操作、理论塔板数为60、回流比为10，塔釜温度为310℃。在塔顶得到富含乙烯基甲苯的物流d，并在塔底得到GLY与二甲基亚砜的混合液。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
对比例1
重复实施例6，区别在于，仅以DMF为萃取剂。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
对比例2
重复实施例6，区别在于，仅以GLY为萃取剂。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
对比例3
重复实施例6，区别在于，萃取剂混合物为N,N-二甲基甲酰胺(DMF)和甘油(GLY)的混合溶液，其中二者质量比为0.67：1。
如上所述计算乙烯基甲苯和C9饱和芳香烃的纯度和收率，结果列在表1中。
表1

由表1可以看出，本发明方法有效分离出乙烯基甲苯和C9饱和芳香烃，获得了改善的纯度和收率。
本申请并不限于上述实施方式中的具体细节，在本申请的技术构思范围内，可以对本申请的技术方案进行多种简单变型，这些简单变型均属于本申请的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本申请对各种可能的组合方式不再另行说明。
此外，本申请的各种不同的实施方式之间也可以进行任意组合，只要其不违背本申请的思想，其同样应当视为本申请所发明的内容。

Claims (13)

  1. 一种分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
    (1)提供含有乙烯基甲苯和C9饱和芳香烃的物流；
    (2)将所述物流与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
  2. 根据权利要求1所述的方法，其中，所述含有乙烯基甲苯和C9饱和芳香烃的物流基本上由或由乙烯基甲苯和C9饱和芳香烃组成；和/或
    所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚；和/或
    所述N,N-二甲基甲酰胺和所述甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。
  3. 根据权利要求2所述的方法，其中，所述萃取剂混合物包含0-50重量％，优选0-20重量％，更优选0-10重量％的辅助萃取剂，并且N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80-100重量％，更优选90-100重量％。
  4. 一种从轻质裂解碳九芳烃中分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的方法，包括以下步骤：
    (1)将轻质裂解碳九芳烃与萃取剂混合物通入萃取精馏塔进行萃取精馏，获得塔顶馏分和塔底馏分，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述塔顶馏分含有C9饱和芳香烃和N,N-二甲基甲酰胺，所述塔底馏分含有乙烯基甲苯和甘油。
  5. 根据权利要求4所述的方法，其进一步包括以下步骤：
    (2)将步骤(1)的塔顶馏分通入到C9饱和芳香烃精制塔进行精制，在塔顶得到N,N-二甲基甲酰胺，并在塔底得到富含C9饱和芳香烃的物流；
    (3)将步骤(1)的塔底馏分通入到乙烯基甲苯精制塔进行精制，在塔顶得到富含乙烯基甲苯的物流，并在塔底得到甘油。
  6. 根据权利要求4所述的方法，其中，所述N,N-二甲基甲酰胺和所述甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1；和/或
    所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚。
  7. 根据权利要求6所述的方法，其中，所述萃取剂混合物包含0-50重量％，优选0-20重量％，更优选0-10重量％的辅助萃取剂，并且N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80-100重量％，更优选90-100重量％。
  8. 根据权利要求4所述的方法，其中，所述萃取剂混合物从萃取精馏塔的上部通入，进料温度为10-30℃；和/或
    所述萃取剂混合物与轻质裂解碳九芳烃的质量流量之比为0.1-1.5，优选为0.1-0.6，更优选为0.2-0.4；和/或
    所述萃取精馏塔的操作条件包括：理论塔板数为50-90块，操作压力为5-20kPa，塔釜温度为250-330℃，回流比为15-25。
  9. 根据权利要求5所述的方法，其中，所述C9饱和芳香烃精制塔的操作条件包括：理论塔板数为40-80块，操作压力为常压，回流比为10-25，塔釜温度为250-265℃；和/或
    所述乙烯基甲苯精制塔的操作条件包括：理论塔板数为50-90块，操作压力为常压，回流比为5-20，塔釜温度为280-380℃。
  10. 根据权利要求5所述的方法，其中，在步骤(2)中，在塔顶得到的N,N-二甲基甲酰胺被返回萃取精馏塔循环使用，并且
    在步骤(3)中，在塔底得到的甘油被返回萃取精馏塔循环使用。
  11. 一种用于通过萃取精馏来分离乙烯基甲苯和C9H12表示的C9饱和芳香烃的萃取剂混合物，其中所述萃取剂混合物包含N,N-二甲基甲酰胺和甘油，所述N,N-二甲基甲酰胺和所述甘油的质量比为0.05-0.5：1，优选为0.06-0.12：1。
  12. 根据权利要求11所述的萃取剂混合物，其中，所述萃取剂混合物包含N,N-二甲基甲酰胺、甘油和辅助萃取剂，其中所述辅助萃取剂选自环丁砜、二甲基亚砜、苯酚。
  13. 根据权利要求12所述的萃取剂混合物，其中，所述萃取剂混合物包含0-50％，优选0-20％，更优选0-10％的辅助萃取剂，并且N,N-二甲基甲酰胺和甘油的总量占萃取剂混合物的50-100重量％，优选80- 100重量％，更优选90-100重量％。
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CN107502386A (zh) 2017-08-30 2017-12-22 南京扬子精细化工有限责任公司 一种裂解碳九经加氢分离获取混合芳烃的方法
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