CN109627139A - Indane separation method in a kind of cracking carbon nine - Google Patents
Indane separation method in a kind of cracking carbon nine Download PDFInfo
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- CN109627139A CN109627139A CN201710934096.2A CN201710934096A CN109627139A CN 109627139 A CN109627139 A CN 109627139A CN 201710934096 A CN201710934096 A CN 201710934096A CN 109627139 A CN109627139 A CN 109627139A
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- 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
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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
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- 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
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Abstract
The present invention relates to indane separation methods in a kind of cracking carbon nine.Pyrolysis c9 by adding hydrogen, by the hydrogenated rear removing of the impurity such as active component therein and sulphur, nitrogen, is obtained hydrocracking carbon nine by the method.By the method for conventional distillation through de- light, Tuo Chonghou, indane component is enriched with hydrocracking carbon nine.It is sent into extractive distillation column rich in indane fraction and mixed solvent, carries out extracting rectifying, extractive distillation column tower bottom obtains indane and mixed solvent, and solvent after indane and regeneration is obtained after solvent recovery tower separates, and wherein solvent can return to extractive distillation column reuse.The present invention isolates 97% or more indane from pyrolysis c9, and indane yield is not less than 80%；Mixed solvent is recycled simultaneously.
Description
Technical field
The present invention relates to a kind of production technologies that indane is obtained from cracking carbon nine, and in particular to a kind of from steam cracking system
The method of indane is obtained in ethylene process in by-product cracking carbon nine.
Background technique
Pyrolysis c9 aromatic hydrocarbons is the by-product of ethylene unit, is cracking naphtha or light diesel, isolates C5 through extracting and evaporate
Divide, the remaining fraction after C6~C8 fraction (hydrogenated production BTX), accounts for about the 10~20% of ethylene total output.
Pyrolysis c9 aromatic fraction composition is extremely complex, and there are about more than 150 kinds, and disperse very much, from the angle of synthesis,
Two classes can be divided into: the active component that one kind can be polymerize, such as styrene and vinyltoluene class, dicyclopentadiene
Deng；Another kind of inactive ingredients, such as alkylbenzene and condensed-nuclei aromatics are used as polymer solvent in the course of the polymerization process.Currently, splitting
The application method of solution C9 aromatic hydrocarbons maturation is to be used directly to production Petropols, and heavy arene therein is as solvent naphtha.Due to splitting
Complicated components in carbon nine are solved, the Petropols color of production is deeper, and added value of product is smaller；There is also colors for solvent oil product
Deeply, the problems such as impurity content is more, need to be promoted by adding hydrogen to promote its quality.
Nine hydrogenation of total effluent technology maturation of carbon is cracked, no matter using one-stage hydrogenation or secondary hydrogenation, it can will be in pyrolysis c9
Active component is converted to inactive ingredients, reduces the impurity such as sulphur, nitrogen in pyrolysis c9, then key component is separated, and can get preferable
Pyrolysis c9 utilizing status.Patent CN201010152296 discloses a kind of production of pyrolysis c9 cut fraction hydrogenation triphen, indane
And aromatic solvent naphtha technique, BTX aromatics are obtained by pretreatment of raw material plus hydrogen and Aromatics Extractive Project, are then obtained by rectifying
The products such as benzene,toluene,xylene, indane and aromatic solvent naphtha improve the comprehensive utilization ratio of pyrolysis c9 fraction, increase additional produce
Value, avoids the waste of resource.But since indane and 1,2,3-trimethylbenzene boiling point are close, pass through the resulting indane purity of conventional distillation
It is lower.
Summary of the invention
The present invention adds the characteristics of indane content is more concentrated after hydrogen, the isolated base rich in indane fraction for pyrolysis c9
On plinth, extracting rectifying is carried out, to obtain the indane of 97% or more purity.This method simple process can obtain 97% or more
Indane can increase the added value of cracking carbon nine, the indane resource in effective use cracking carbon nine.
Technical solution proposed by the present invention are as follows: hydrocracking C9 is sent into lightness-removing column, removes C8 and following light component, lightness-removing column
Tower top obtains C8 and following light component, and tower bottom obtains C9 and the above component；C9 and above group are distributed into weight-removing column, remove C10 and
The above component, weight-removing column tower top obtain C9 component, and tower bottom obtains C10 and the above component.C9 component and solvent are sent into extracting rectifying
Tower carries out extracting rectifying, and extracting rectifying column overhead obtains C9, and tower bottom obtains indane and solvent, and indane and solvent are through solvent recovery
The indane and solvent of 97% or more purity are obtained after tower separation, wherein solvent can return to extractive distillation column reuse.
Specifically, the present invention relates to the contents of following aspect:
In above-mentioned technical proposal, pyrolysis c9 to be separated derives from preparing ethylene by steam cracking device, isolates C6~C8 group
Obtained component after point.Removing, obtains hydrocracking carbon nine after the impurity such as active component and sulphur, nitrogen are hydrogenated in pyrolysis c9.
C8 and following components, C9 component, C10 and the above component are mainly contained in hydrocracking carbon nine, boiling point difference is larger between them,
Therefore it can be separated by the method for conventional distillation.Hydrocracking carbon nine, which passes through, takes off light, Tuo Chonghou, main in isolated C9 component
For trimethylbenzene, indane and a small amount of bicyclic pentane.
In above-mentioned technical proposal, indane and trimethylbenzene are separated since boiling point is close using extraction rectifying method,
Extractant used is the mixed solvent of sulfolane and N-Methyl pyrrolidone (NMP) composition.Mixed solvent can be improved trimethylbenzene with
Relative volatility between indane, to realize that isolated purity is 97% indane.Mixed solvent sulfolan and NMP matter
Amount is than being 9: 1~1: 9.Preferably mixed solvent sulfolan and NMP mass ratio are 4: 6~6: 4
In above-mentioned technical proposal, the extractive distillation column, number of theoretical plate is 60~100 pieces, reflux ratio is 2~8, solvent
It is 1~10 than (the ratio between mixed solvent amount and inlet amount).After extracting rectifying, extractive distillation column tower bottom indane content up to 97% with
Upper (being free of solvent), indane yield are 80% or more.Extractive distillation column preferably number of theoretical plate is 80~100 pieces, reflux ratio 5
~6, solvent ratio is 3~5.
In above-mentioned technical proposal, the solvent recovery tower is vacuum rectification tower, and number of theoretical plate is 30~60 pieces, reflux ratio
It is 2~5, after rectification under vacuum, the top of the distillation column produces 97% or more indane, and tower reactor extraction mixed solvent can reenter extraction
It takes in rectifying column and reuses.
Beneficial effect
Compared with the prior art, the advantages of the present invention are as follows can be isolated from pyrolysis c9 with the method for rectifying 97% with
On indane, and indane yield be not less than 80%；Extractant is recycled simultaneously, does not generate environmentally harmful substance, realizes
The effective use of indenes resource in pyrolysis c9.
Specific embodiment
Detailed description of the preferred embodiments below, it should be noted however that protection of the invention
Range is not limited to these specific embodiments, but is determined by claims.
The pairs of separating resulting influence of cracking nine raw material group of carbon is smaller, and embodiment becomes representative with typical case's group and analyzed, and splits
Solve the typical composition of carbon nine are as follows:
Embodiment 1
Pyrolysis c9, by the hydrogenated rear removing of the impurity such as active component therein and sulphur, nitrogen, obtains hydrocracking by adding hydrogen
Carbon nine.Hydrocracking carbon nine is by the method for conventional distillation through de- light, Tuo Chonghou, and indane component is enriched with, main material
Composition are as follows: trimethylbenzene 13.2%, indane 86.3%, bicyclic pentane 0.4%, other components 0.1%, the indane rate of recovery are 96%.
It will be enriched in indane fraction and solvent N-methyl pyrilidone (NMP) and sulfolane mixed solvent be sent into extractive distillation column
In, extractive distillation column number of theoretical plate is 80, and the charging of indane fraction is the 35th block of column plate, and mixed solvent charging is the 4th block of column plate,
Reflux ratio is 5, and solvent ratio is 3, NMP and sulfolane mass ratio is 6: 4.Tower reactor obtains mixed solvent and indenes after extracting rectifying
Full, indane purity is 98.02% (disregarding mixed solvent amount), and the indane rate of recovery is 86%.Indane and mixed solvent, which are sent into, to depressurize
Indane purification is carried out in rectifying column, vacuum rectification tower number of theoretical plate is 50, reflux ratio 3, tower reactor pressure 22KPa.Through decompression point
From rear, indane purity is 98.02%.
Embodiment 2
Pyrolysis c9, by the hydrogenated rear removing of the impurity such as active component therein and sulphur, nitrogen, obtains hydrocracking by adding hydrogen
Carbon nine.Hydrocracking carbon nine is by the method for conventional distillation through de- light, Tuo Chonghou, and indane component is enriched with, main material
Composition are as follows: trimethylbenzene 13.2%, indane 86.3%, bicyclic pentane 0.4%, other components 0.1%, the indane rate of recovery are 96%.
It will be enriched in indane fraction and solvent N-methyl pyrilidone (NMP) and sulfolane mixed solvent be sent into extractive distillation column
In, extractive distillation column number of theoretical plate is 100, and the charging of indane fraction is the 45th block of column plate, and mixed solvent charging is the 4th piece of tower
Plate, reflux ratio 2, solvent ratio is 1, NMP and sulfolane mass ratio is 9: 1.After extracting rectifying tower reactor obtain mixed solvent and
Indane, indane purity are 97.03% (disregarding mixed solvent amount), and the indane rate of recovery is 86%.Indane subtracts with mixed solvent feeding
It presses and carries out indane purification in rectifying column, vacuum rectification tower number of theoretical plate is 30, reflux ratio 5, tower reactor pressure 30KPa.Through depressurizing
After separation, indane purity is 97.03%.
Embodiment 3
Pyrolysis c9, by the hydrogenated rear removing of the impurity such as active component therein and sulphur, nitrogen, obtains hydrocracking by adding hydrogen
Carbon nine.Hydrocracking carbon nine is by the method for conventional distillation through de- light, Tuo Chonghou, and indane component is enriched with, main material
Composition are as follows: trimethylbenzene 13.2%, indane 86.3%, bicyclic pentane 0.4%, other components 0.1%, the indane rate of recovery are 96%.
It will be enriched in indane fraction and solvent N-methyl pyrilidone (NMP) and sulfolane mixed solvent be sent into extractive distillation column
In, extractive distillation column number of theoretical plate is 60, and the charging of indane fraction is the 25th block of column plate, and mixed solvent charging is the 4th block of column plate,
Reflux ratio is 8, and solvent ratio is 10, NMP and sulfolane mass ratio is 1: 9.Tower reactor obtains mixed solvent and indenes after extracting rectifying
Full, indane purity is 97.06% (disregarding mixed solvent amount), and the indane rate of recovery is 84%.Indane and mixed solvent, which are sent into, to depressurize
Indane purification is carried out in rectifying column, vacuum rectification tower number of theoretical plate is 60, reflux ratio 2, tower reactor pressure 100KPa.Through decompression point
From rear, indane purity is 97.06%.
Embodiment 4
Pyrolysis c9, by the hydrogenated rear removing of the impurity such as active component therein and sulphur, nitrogen, obtains hydrocracking by adding hydrogen
Carbon nine.Hydrocracking carbon nine is by the method for conventional distillation through de- light, Tuo Chonghou, and indane component is enriched with, main material
Composition are as follows: trimethylbenzene 13.2%, indane 86.3%, bicyclic pentane 0.4%, other components 0.1%, the indane rate of recovery are 96%.
It will be enriched in indane fraction and solvent N-methyl pyrilidone (NMP) and sulfolane mixed solvent be sent into extractive distillation column
In, extractive distillation column number of theoretical plate is 80, and the charging of indane fraction is the 35th block of column plate, and mixed solvent charging is the 4th block of column plate,
Reflux ratio is 5, and solvent ratio is 5, NMP and sulfolane mass ratio is 4: 6.Tower reactor obtains mixed solvent and indenes after extracting rectifying
Full, indane purity is 98.05% (disregarding mixed solvent amount), and the indane rate of recovery is 86%.Indane and mixed solvent, which are sent into, to depressurize
Indane purification is carried out in rectifying column, vacuum rectification tower number of theoretical plate is 50, reflux ratio 3, tower reactor pressure 22KPa.Through decompression point
From rear, indane purity is 98.05%.
Although a specific embodiment of the invention is described in detail above in conjunction with the embodiments, need to refer to
Out, the scope of protection of the present invention is not limited by these specific embodiments, but is determined by claims.This
Field technical staff can carry out these embodiments in the range of not departing from technical idea and purport of the invention appropriate
Change, and the embodiment after these changes is obviously also included within protection scope of the present invention.
Claims (5)
1. indane separation method in a kind of cracking carbon nine, it is characterised in that: pyrolysis c9 obtains hydrocracking carbon nine by adding hydrogen,
Hydrocracking carbon nine is by the method for conventional distillation through de- light, Tuo Chonghou, and indane component is enriched with, main material are as follows: three
Toluene, indane, bicyclic pentane, will be enriched in indane fraction and N-Methyl pyrrolidone and sulfolane mixed solvent is sent into extracting rectifying
In tower, mixed solvent sulfolan and NMP mass ratio are 9: 1~1: 9, the extractive distillation column, number of theoretical plate is 60~
100 pieces, reflux ratio be 2~8, the mass ratio of mixed solvent amount and inlet amount is 1~10；
Tower reactor obtains mixed solvent and indane after extracting rectifying, and indane and mixed solvent, which are sent into vacuum rectification tower, carries out indane
Purification, vacuum rectification tower number of theoretical plate are 30~60 pieces, and reflux ratio is 3~5,20~100KPa of tower reactor pressure.
2. indane separation method in cracking carbon nine according to claim 1, it is characterised in that: the pyrolysis c9 derives from
Preparing ethylene by steam cracking device isolates obtained component after C6~C8 component, and active component and sulphur, nitrogen etc. are miscellaneous in pyrolysis c9
Removing, obtains hydrocracking carbon nine after matter is hydrogenated.
3. indane separation method in cracking carbon nine according to claim 1, it is characterised in that: mixed solvent sulfolan with
NMP mass ratio is 4: 6~6: 4.
4. indane separation method in cracking carbon nine according to claim 1, it is characterised in that: the extractive distillation column
Number of theoretical plate is 80~100 pieces, and reflux ratio is 5~6, and the mass ratio of mixed solvent amount and inlet amount is 3~5.
5. indane separation method in cracking carbon nine according to claim 1, it is characterised in that: the solvent recovery tower is
Vacuum rectification tower, number of theoretical plate are 50 pieces, reflux ratio 3, tower reactor pressure 20KPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710934096.2A CN109627139A (en) | 2017-10-09 | 2017-10-09 | Indane separation method in a kind of cracking carbon nine |
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| CN201710934096.2A CN109627139A (en) | 2017-10-09 | 2017-10-09 | Indane separation method in a kind of cracking carbon nine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195613A (en) * | 2020-09-18 | 2022-03-18 | 宝武炭材料科技有限公司 | Indene extractive distillation purification method |
| CN114315792A (en) * | 2020-09-30 | 2022-04-12 | 宝武炭材料科技有限公司 | Method for enriching thianaphthene from mixture of thianaphthene and naphthalene by solvent crystallization coupled extraction rectification method |
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| US2413253A (en) * | 1944-02-09 | 1946-12-24 | United Gas Improvement Co | Purification of indene |
| CN101575261A (en) * | 2009-06-16 | 2009-11-11 | 南京师范大学 | Method for extracting, rectifying and separating pseudocumene and indane |
| CN101824336A (en) * | 2010-04-22 | 2010-09-08 | 中国寰球工程公司辽宁分公司 | Technique for producing terphenyl, indane and aromatics solvent oil by cracking C9 fraction and hydrogenation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195613A (en) * | 2020-09-18 | 2022-03-18 | 宝武炭材料科技有限公司 | Indene extractive distillation purification method |
| CN114315792A (en) * | 2020-09-30 | 2022-04-12 | 宝武炭材料科技有限公司 | Method for enriching thianaphthene from mixture of thianaphthene and naphthalene by solvent crystallization coupled extraction rectification method |
| CN114315792B (en) * | 2020-09-30 | 2023-06-23 | 宝武碳业科技股份有限公司 | Method for enriching thiaindene from mixture of thiaindene and naphthalene by solvent crystallization coupling extraction rectification method |
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