CN105461501B - Between C9 mixture extracting rectifyings, the saline extraction agent of p-methyl-ethylbenzene and separation method - Google Patents
Between C9 mixture extracting rectifyings, the saline extraction agent of p-methyl-ethylbenzene and separation method Download PDFInfo
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Abstract
The present invention relates to a kind of C9Between mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene and separation method, mainly solve C9In the middle of aromatic hydrocarbons mixture, p-methyl-ethylbenzene be difficult to the technical problem that separates.The present invention is by using the extractant in using salicylate as saline extraction agent, and rhodanate is as the salt in saline extraction agent, by C9Aromatic hydrocarbons mixture introduces tower top and sets the heavies removal column of hydrops tank to carry out batch fractionating, tower reactor produces pseudocumene and 1,2,3-trimethylbenzene, tower top stream stock introduces extractive distillation column and carries out extracting rectifying, from between overhead extraction, p-methyl-ethylbenzene, tower reactor stream stock enters solvent recovery tower, and tower top obtains o-methylethylbenzene and mesitylene, the technical scheme that the saline extraction agent that tower reactor is obtained is recycled, above mentioned problem is preferably resolved, C is can be applied to9In aromatic hydrocarbons mixture separation field.
Description
Technical field
The invention belongs to chemical separating field, in particular it relates to a kind of from C9In aromatic hydrocarbons mixture between extracting rectifying, to first
The saline extraction agent of ethylbenzene and separation method.
Background technology
Between, p-methyl-ethylbenzene dehydrogenation product there is extensive use.Meanwhile, p-methyl-ethylbenzene still synthesize 1-chloro-4-methyl-benzene
With the good raw material for aoxidizing methyl benzoic acid processed.However, C9The boiling point of each component is sufficiently close in aromatic hydrocarbons mixture, using routine
Method is difficult to C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.
At present, the main method using precise distillation and benzene with catalytic rectifying is from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.
Document CN200810225604.0 discloses a kind of separation C9The method of aromatic hydrocarbons.The tower separation process of this method two, takes off
Weight tower pressurized operation, lightness-removing column decompression operation.This method belongs to precise distillation method, only by improve weight-removing column operating pressure and
Reducing dehydrogenation tower operating pressure just can isolated, p-methyl-ethylbenzene mixture.But number of theoretical plate needed for this method and reflux ratio
It is higher.
Document CN102399125A discloses a kind of from C9Compartment, the benzene with catalytic rectifying side of p-methyl-ethylbenzene in aromatic hydrocarbons mixture
Method.This method uses a kind of be used as in acetonitrile or propionitrile to urge agent, changes both by changing the surface nature of thing system
Relative volatility.This method operating procedure is similar with extracting rectifying, but urges agent to be different from extractant.
In order to solve existing C9In the middle of aromatic hydrocarbons mixture, the technical problem of p-methyl-ethylbenzene separation, exploitation is a kind of from C9Aromatic hydrocarbons is mixed
Compartment, the saline extraction agent of p-methyl-ethylbenzene and extraction rectifying method are necessary in compound.
The content of the invention
One of technical problems to be solved by the invention are C9In the middle of aromatic hydrocarbons mixture, p-methyl-ethylbenzene be difficult to separate, propose
A kind of C9Between aromatic hydrocarbons mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene.Can be high using the saline extraction agent of the present invention
Effect realizes C9Between aromatic hydrocarbons mixture extracting rectifying, p-methyl-ethylbenzene.The characteristics of technical scheme has extractant low toxicity, consumption is small.
The two of the technical problems to be solved by the invention are using the saline extraction agent described in one of technical problem solved
To C9In the middle of aromatic hydrocarbons mixture, p-methyl-ethylbenzene carry out extracting rectifying method, can be preferable using technical scheme
Compartment, p-methyl-ethylbenzene, have the advantages that separating effect is high.
To solve one of above-mentioned technical problem, the technical solution adopted by the present invention is as follows：A kind of C9Aromatic hydrocarbons mixture is extracted
Between rectifying, the saline extraction agent of p-methyl-ethylbenzene, wherein extractant is salicylate, and the salt of saline extraction agent is rhodanate.
In above-mentioned technical proposal salicylate in gaultherolin, salethyl and isopropyl salicylate at least
One kind, preferably gaultherolin；Rhodanate is selected from potassium rhodanide or/and sodium sulfocyanate, preferably potassium rhodanide.
In above-mentioned technical proposal, in terms of saline extraction agent gross mass, wherein, the mass fraction of impurity is more than or equal to 0 and small
In equal to 2%, in terms of the gross mass of salicylate and rhodanate in saline extraction agent, wherein, the mass fraction of salicylate
More than or equal to 90% and less than or equal to 99%, the mass fraction of rhodanate is more than or equal to 1% and less than or equal to 10%.
In above-mentioned technical proposal, the saline extraction agent and C9The quality of aromatic hydrocarbons mixture is 0.5~0.8 than scope.
In above-mentioned technical proposal, technical scheme salicylate and the mass ratio of rhodanate preferably are (96~93):(7
~4), saline extraction agent and C9The quality of aromatic hydrocarbons mixture is 0.7~0.8 than scope.
In above-mentioned technical proposal, saline extraction agent is preferably gaultherolin, salethyl, potassium rhodanide and thiocyanic acid
The mixed extractant of sodium, wherein, the quality of gaultherolin, salethyl, potassium rhodanide and sodium sulfocyanate in extractant
Than for (47~53):(47~43):(3~2):(3~2), extractant and C9The mass ratio of aromatic hydrocarbons mixture is 0.76~0.8.
To solve the two of above-mentioned technical problem, the technical solution adopted by the present invention is as follows：Using the above saline extraction
Agent, from C9Compartment, the extraction rectifying method of p-methyl-ethylbenzene comprise the following steps in aromatic hydrocarbons mixture：
By C9Aromatic hydrocarbons mixture introduces heavies removal column and carries out batch fractionating, and heavies removal column overhead sets hydrops
Tank, heavies removal column tower reactor extraction pseudocumene and 1,2,3-trimethylbenzene, overhead stream introduce extracting rectifying, saline extraction from bottom
Agent logistics introduces extractive distillation column, both cross-flows contact from top；Between extractive distillation column overhead extraction, p-methyl-ethylbenzene, tower reactor stream
Stock enters solvent recovery tower；Solvent recovery tower overhead extraction o-methylethylbenzene and mesitylene, tower reactor extraction saline extraction agent logistics,
Saline extraction agent logistics introduces extractive distillation column top and recycled.
In above-mentioned extraction rectifying method, the hydrops tank that heavies removal column overhead is set is single hydrops tank or biproduct flow container；
Heavies removal column number of theoretical plate is more than or equal to 20 pieces and less than or equal to 40 pieces, and tower top mass reflux ratio is more than or equal to 1 and is less than
Equal to 4, tower top operating pressure is more than or equal to 0.06MPa and less than or equal to 0.12MPa；Extractive distillation column number of theoretical plate is more than or equal to
60 pieces and less than or equal to 80 pieces, tower top mass reflux ratio is more than or equal to 2 and less than or equal to 4, and tower top operating pressure is more than or equal to
0.08MPa and less than or equal to 0.12MPa；Solvent recovery tower number of theoretical plate is more than or equal to 10 pieces and less than or equal to 20 pieces, tower top matter
Measure reflux ratio and be more than or equal to 1 and less than or equal to 2, tower top operating pressure is more than or equal to 0.08MPa and less than or equal to 0.12MPa.Respectively
Tower is operated preferably under 0.1MPa.
In above-mentioned technical proposal, C used9Aromatic hydrocarbons mixture derives from the reaction product of toluene and the benzene of ethene system first and second, with C9
Aromatic hydrocarbons mixture gross mass meter, wherein, C9The weight/mass percentage composition of component was more than or equal to 0 and less than or equal to 10% in the past, a first
The weight/mass percentage composition sum of ethylbenzene and p-methyl-ethylbenzene is more than or equal to 65% and less than or equal to 85%, o-methylethylbenzene and mesitylene
Weight/mass percentage composition sum be more than or equal to 1% and less than or equal to 5%.
The saline extraction agent of salicylate and rhodanate is included using the present invention, by C9Aromatic hydrocarbons mixture introduces restructuring
Removing tower is divided to carry out batch fractionating, heavies removal column overhead sets hydrops tank, heavies removal column tower reactor extraction pseudocumene
And 1,2,3-trimethylbenzene, overhead stream from bottom introduce extracting rectifying, saline extraction agent logistics from top introduce extractive distillation column, both
Cross-flow is contacted；Between extractive distillation column overhead extraction, p-methyl-ethylbenzene, tower reactor stream stock enters solvent recovery tower；Solvent recovery column overhead
O-methylethylbenzene and mesitylene are produced, tower reactor extraction saline extraction agent logistics, saline extraction agent logistics is introduced on extractive distillation column
The technical scheme that portion is recycled, has been obtained between product, p-methyl-ethylbenzene yield 90.87%, between product, total matter of p-methyl-ethylbenzene
Gauge, p-methyl-ethylbenzene gross mass percentage composition 98.58%, the effect of o-methylethylbenzene weight/mass percentage composition 0.40%.
Brief description of the drawings
Fig. 1 is C of the invention9Between aromatic hydrocarbons mixture extracting rectifying, the separating technology schematic flow sheet of p-methyl-ethylbenzene.Fig. 1
In 1 be heavies removal column, 2 be extractive distillation column, and 3 be solvent recovery tower, and 4 be C9Aromatic hydrocarbons mixture logistics, 5 is de- for heavy constituent
Except first piece of theoretical plate of tower, 6 be tower top hydrops tank, and 7 be heavies removal column tower reactor logistics, and 8 be heavies removal column overhead materials
Stream, 9 be fresh saline extraction agent logistics, and 10 be extracting rectifying column overhead stream, and 11 be extractive distillation column tower reactor logistics, and 12 be molten
Column overhead stream is reclaimed in agent, and 13 be that saline extraction agent circulates logistics.C9Aromatic hydrocarbons mixture 4 is introduced from the middle part of heavies removal column 1,
Heavies removal column tower reactor logistics 7 containing pseudocumene and 1,2,3-trimethylbenzene is produced from the tower reactor of heavies removal column 1, other C9Component
After tower top hydrops tank 6 heavies removal column 1, tower top hydrops tank 6 are back to from the top of first piece of theoretical plate of heavies removal column 5
After middle fluid product purity is qualified, enter extractive distillation column 2 from bottom as heavies removal column overhead stream 8；In extraction essence
Evaporate in tower 2 fresh saline extraction agent 9 to introduce from tower top, and the cross-flow of logistics 8 contact, between a part, p-methyl-ethylbenzene product is from extraction
Take in the overhead stream 10 of rectifying column 2 and produce, another part is back to extractive distillation column；Containing o-methylethylbenzene and mesitylene and
The extractive distillation column tower reactor logistics 11 of extractant introduces solvent recovery tower 3 from the extraction of the tower reactor of extractive distillation column 2；Solvent recovery tower 3
Solvent recovery column overhead stream 12 of the overhead extraction part containing o-methylethylbenzene and mesitylene, another part is back to solvent and returned
Tower is received, the Posterior circle of solvent recovery tower tower reactor extraction saline extraction agent logistics 13 is circulated to the top of extractive distillation column 2 to be used.
Embodiment
With reference to embodiment, the method for the present invention is further illustrated, but the method for the present invention and more than that.
The raw material of embodiment comes from the reaction product of toluene and the benzene of ethylene reaction system first and second.Toluene and ethylene reaction first
The reaction product of ethylbenzene removes most of toluene, ethylbenzene and dimethylbenzene after rectifying, resultant product as embodiment raw material, its
Main composition is C9 aromatic hydrocarbons mixtures.
Between product, the yield of p-methyl-ethylbenzene calculated in such a way：
【Embodiment 1】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Saline extraction agent is selected with matter
99 parts of the gaultherolin of gauge and 1 part of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.5.20 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 1；Extractive distillation column number of theoretical plate
60 pieces, reflux ratio in mass is 2；10 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 1；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 88.96%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 96.17%, the weight/mass percentage composition of o-methylethylbenzene is 0.78%.
【Embodiment 2】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Saline extraction agent is selected with matter
90 parts of the gaultherolin of gauge and 10 parts of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.5.20 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 1；Extractive distillation column number of theoretical plate
60 pieces, reflux ratio in mass is 2；10 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 1；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 89.36%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 96.28%, the weight/mass percentage composition of o-methylethylbenzene is 0.77%.
【Embodiment 3】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Saline extraction agent is selected with matter
2 parts of 95 parts of gaultherolin, 3 parts of potassium rhodanide in mass and the sodium sulfocyanate in mass of gauge.Saline extraction
Agent gross mass and C9The ratio of aromatic hydrocarbons mixture gross mass is 0.5.20 pieces of heavies removal column number of theoretical plate, time in mass
Stream is than being 1；60 pieces of extractive distillation column number of theoretical plate, reflux ratio in mass is 2；10 pieces of solvent recovery tower number of theoretical plate, with
The reflux ratio of quality meter is 1；Each column overhead pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 90.03%.With
Between product, the gross mass meter of p-methyl-ethylbenzene, the weight/mass percentage composition of p-methyl-ethylbenzene be 97.23%, the quality hundred of o-methylethylbenzene
It is 0.71% to divide content.
【Embodiment 4】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Saline extraction agent is selected with matter
99 parts of the salethyl of gauge and 1 part of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.5.20 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 1；Extractive distillation column number of theoretical plate
60 pieces, reflux ratio in mass is 2；10 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 1；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 88.40%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 96.05%, the weight/mass percentage composition of o-methylethylbenzene is 0.84%.
【Embodiment 5】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Saline extraction agent is selected with matter
90 parts of the salethyl of gauge and 10 parts of sodium sulfocyanate in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.5.20 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 1；Extractive distillation column number of theoretical plate
60 pieces, reflux ratio in mass is 2；10 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 1；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 87.04%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 95.34%, the weight/mass percentage composition of o-methylethylbenzene is 0.93%.
【Embodiment 6~15】
Raw material composition and operating condition with reference to embodiment 1~5 is constant, only changes the species and composition of saline extraction agent,
Between obtaining, p-methyl-ethylbenzene product.
The extractant species and composition of embodiment 1~15 and, the yield of p-methyl-ethylbenzene product and quality index such as table
1.In table 1, A1 represents gaultherolin, and A2 represents salethyl, and A3 represents isopropyl salicylate, and B1 represents potassium rhodanide,
B2 represents sodium sulfocyanate.
Table 1
【Embodiment 16】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Saline extraction agent is selected with matter
99 parts of the gaultherolin of gauge and 1 part of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.8.40 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 4；Extractive distillation column number of theoretical plate
80 pieces, reflux ratio in mass is 4；20 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 2；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 89.42%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 98.20%, the weight/mass percentage composition of o-methylethylbenzene is 0.51%.
【Embodiment 17】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Saline extraction agent is selected with matter
90 parts of the gaultherolin of gauge and 10 parts of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.8.40 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 4；Extractive distillation column number of theoretical plate
80 pieces, reflux ratio in mass is 4；20 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 2；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 89.76%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 98.28%, the weight/mass percentage composition of o-methylethylbenzene is 0.49%.
【Embodiment 18】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Saline extraction agent is selected with matter
2 parts of 95 parts of gaultherolin, 3 parts of potassium rhodanide in mass and the sodium sulfocyanate in mass of gauge.Saline extraction
Agent gross mass and C9The ratio of aromatic hydrocarbons mixture gross mass is 0.8.40 pieces of heavies removal column number of theoretical plate, backflow in mass
Than for 4；80 pieces of extractive distillation column number of theoretical plate, reflux ratio in mass is 4；20 pieces of solvent recovery tower number of theoretical plate, with matter
The reflux ratio of gauge is 2；Each column overhead pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 90.74%.To produce
Between product, the gross mass meter of p-methyl-ethylbenzene, the weight/mass percentage composition of p-methyl-ethylbenzene be 98.56%, the quality percentage of o-methylethylbenzene
Content is 0.43%.
【Embodiment 19】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Saline extraction agent is selected with matter
99 parts of the salethyl of gauge and 1 part of potassium rhodanide in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.8.40 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 4；Extractive distillation column number of theoretical plate
80 pieces, reflux ratio in mass is 4；20 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 2；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 89.16%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 98.13%, the weight/mass percentage composition of o-methylethylbenzene is 0.58%.
【Embodiment 20】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Saline extraction agent is selected with matter
90 parts of the salethyl of gauge and 10 parts of sodium sulfocyanate in mass.Saline extraction agent gross mass and C9Aromatic hydrocarbons mixture is total
The ratio of quality is 0.8.40 pieces of heavies removal column number of theoretical plate, reflux ratio in mass is 4；Extractive distillation column number of theoretical plate
80 pieces, reflux ratio in mass is 4；20 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 2；Each column overhead
Pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is 86.62%.Between product, in terms of the gross mass of p-methyl-ethylbenzene,
Between, the weight/mass percentage composition of p-methyl-ethylbenzene be 97.41%, the weight/mass percentage composition of o-methylethylbenzene is 0.64%.
【Embodiment 21~30】
Raw material composition and operating condition with reference to embodiment 16~20 is constant, only changes the species and group of saline extraction agent
Into between obtaining, p-methyl-ethylbenzene product.
The extractant species and composition of embodiment 16~30 and, the yield of p-methyl-ethylbenzene product and quality index such as table
2.In table 2, A1 represents gaultherolin, and A2 represents salethyl, and A3 represents isopropyl salicylate, and B1 represents potassium rhodanide,
B2 represents sodium sulfocyanate.
Table 2
【Comparative example 1】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Without using extractant.Restructuring
Divide 20 pieces of removing tower number of theoretical plate, reflux ratio in mass is 1；160 pieces of extractive distillation column number of theoretical plate, time in mass
Stream is than being 20；10 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 1；Each column overhead pressure is 0.1MPa.Obtain
Between product, the yield of p-methyl-ethylbenzene be 58.01%.Between product, in terms of the gross mass of p-methyl-ethylbenzene, the quality of p-methyl-ethylbenzene
Percentage composition is 94.45%, and the weight/mass percentage composition of o-methylethylbenzene is 0.89%.
【Comparative example 2】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Without using extractant.Restructuring
Divide 40 pieces of removing tower number of theoretical plate, reflux ratio in mass is 4；160 pieces of extractive distillation column number of theoretical plate, time in mass
Stream is than being 20；20 pieces of solvent recovery tower number of theoretical plate, reflux ratio in mass is 2；Each column overhead pressure is 0.1MPa.Obtain
Between product, the yield of p-methyl-ethylbenzene be 57.44%.Between product, in terms of the gross mass of p-methyl-ethylbenzene, the quality of p-methyl-ethylbenzene
Percentage composition is 95.61%, and the weight/mass percentage composition of o-methylethylbenzene is 0.76%.
【Comparative example 3】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 1.06%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 82.80% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 1.57%.Extractant selects salicylic acid first
Ester.Extractant gross mass and C9The ratio of aromatic hydrocarbons mixture gross mass is 1.5.20 pieces of heavies removal column number of theoretical plate, with quality
The reflux ratio of meter is 1；60 pieces of extractive distillation column number of theoretical plate, reflux ratio in mass is 2；Solvent recovery tower number of theoretical plate 10
Block, reflux ratio in mass is 1；Each column overhead pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is
87.84%.Between product, in terms of the gross mass of p-methyl-ethylbenzene, the weight/mass percentage composition of p-methyl-ethylbenzene be 96.03%, adjacent first
The weight/mass percentage composition of ethylbenzene is 0.83%.
【Comparative example 4】
Flow shown in reference picture 1, from C9Compartment, p-methyl-ethylbenzene in aromatic hydrocarbons mixture.With C9Aromatic hydrocarbons mixture gross mass
Meter, C9In aromatic hydrocarbons mixture, C9The weight/mass percentage composition of preceding component is 8.36%, the gross mass hundred of m-methyl ethylbenzene and p-methyl-ethylbenzene
It is 67.88% to divide content, and the gross mass percentage composition of mesitylene and o-methylethylbenzene is 4.51%.Extractant selects salicylic acid first
Ester.Extractant gross mass and C9The ratio of aromatic hydrocarbons mixture gross mass is 4.40 pieces of heavies removal column number of theoretical plate, in mass
Reflux ratio be 4；80 pieces of extractive distillation column number of theoretical plate, reflux ratio in mass is 4；Solvent recovery tower number of theoretical plate 20
Block, reflux ratio in mass is 2；Each column overhead pressure is 0.1MPa.Obtain between product, the yield of p-methyl-ethylbenzene is
87.89%.Between product, in terms of the gross mass of p-methyl-ethylbenzene, the weight/mass percentage composition of p-methyl-ethylbenzene be 97.80%, neighbour first and second
The weight/mass percentage composition of benzene is 0.56%.
Claims (9)
1. a kind of C9Between mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene, it is characterised in that the saline extraction agent
Main extractant is salicylate, and the salt of the saline extraction agent is rhodanate；With salicylate and sulphur in saline extraction agent
The gross mass meter of cyanate, wherein, the mass fraction of salicylate is more than or equal to 90% and less than or equal to 99%, rhodanate
Mass fraction is more than or equal to 1% and less than or equal to 10%.
2. C according to claim 19Between mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene, it is characterised in that institute
State at least one of the salicylate in gaultherolin, salethyl and isopropyl salicylate, the rhodanate choosing
From potassium rhodanide or/and sodium sulfocyanate.
3. C according to claim 19Between mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene, it is characterised in that with
Saline extraction agent gross mass meter, wherein, the mass percent of impurity is more than or equal to 0 and less than or equal to 2%.
4. C according to claim 19Between mixture extracting rectifying, the saline extraction agent of p-methyl-ethylbenzene, it is characterised in that institute
State saline extraction agent and C9The mass ratio of aromatic hydrocarbons mixture is more than or equal to 0.5 and less than or equal to 0.8.
5. a kind of C9Between mixture extracting rectifying, the separation method of p-methyl-ethylbenzene, salt is added using any one in claim 1-4
Extractant, it is characterised in that this method comprises the following steps：
By C9Aromatic hydrocarbons mixture introduces heavies removal column and carries out batch fractionating, and heavies removal column overhead sets hydrops tank, restructuring
Divide removing tower tower reactor extraction pseudocumene and 1,2,3-trimethylbenzene, overhead stream introduces extractive distillation column, saline extraction agent thing from bottom
Stream introduces extractive distillation column, both cross-flows contact from top；Between extractive distillation column overhead extraction, p-methyl-ethylbenzene, tower reactor logistics enters
Enter solvent recovery tower；Solvent recovery tower overhead extraction o-methylethylbenzene and mesitylene, tower reactor extraction saline extraction agent logistics, plus salt
Extractant stream introduces extractive distillation column top and recycled.
6. C according to claim 59Between mixture extracting rectifying, the separation method of p-methyl-ethylbenzene, it is characterised in that restructuring
It is single hydrops tank or biproduct flow container to divide the removing hydrops tank that column overhead is set.
7. C according to claim 59Between mixture extracting rectifying, the separation method of p-methyl-ethylbenzene, it is characterised in that it is described
Heavies removal column number of theoretical plate is more than or equal to 20 pieces and less than or equal to 40 pieces, and tower top mass reflux ratio is more than or equal to 1 and is less than
Equal to 4, tower top operating pressure is more than or equal to 0.06MPa and less than or equal to 0.12MPa；The extractive distillation column number of theoretical plate is more than
Equal to 60 pieces and less than or equal to 80 pieces, tower top mass reflux ratio is more than or equal to 2 and less than or equal to 4, and tower top operating pressure is more than etc.
In 0.08MPa and less than or equal to 0.12MPa；The solvent recovery tower number of theoretical plate is more than or equal to 10 pieces and less than or equal to 20 pieces,
Tower top mass reflux ratio is more than or equal to 1 and less than or equal to 2, and tower top operating pressure is more than or equal to 0.08MPa and is less than or equal to
0.12MPa。
8. C according to claim 59Between mixture extracting rectifying, the separation method of p-methyl-ethylbenzene, it is characterised in that it is described
Heavies removal column, extractive distillation column and solvent recovery tower are operated under 0.1MPa.
9. C according to claim 59Between mixture extracting rectifying, the separation method of p-methyl-ethylbenzene, it is characterised in that it is used
C9Aromatic hydrocarbons mixture derives from the reaction product of toluene and the benzene of ethene system first and second, with C9Aromatic hydrocarbons mixture gross mass meter, wherein, C9
The weight/mass percentage composition of component was more than or equal to 0 and less than or equal to 10% in the past, and the quality percentage of m-methyl ethylbenzene and p-methyl-ethylbenzene contains
Measure sum and be more than or equal to 65% and less than or equal to 85%, the weight/mass percentage composition sum of o-methylethylbenzene and mesitylene is more than or equal to
1% and less than or equal to 5%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538185A (en) * | 2009-04-14 | 2009-09-23 | 中国石化扬子石油化工有限公司 | Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation |
| CN102924211A (en) * | 2011-08-08 | 2013-02-13 | 中国石油化工股份有限公司 | Solvent composition for separating m-methyl-ethylbenzene from p-methyl-ethylbenzene by extractive distillation and extractive distillation method |
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2014
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538185A (en) * | 2009-04-14 | 2009-09-23 | 中国石化扬子石油化工有限公司 | Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation |
| CN102924211A (en) * | 2011-08-08 | 2013-02-13 | 中国石油化工股份有限公司 | Solvent composition for separating m-methyl-ethylbenzene from p-methyl-ethylbenzene by extractive distillation and extractive distillation method |
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