CN109627140A - A kind of mesitylene extraction and rectification separation method - Google Patents
A kind of mesitylene extraction and rectification separation method Download PDFInfo
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- CN109627140A CN109627140A CN201710933993.1A CN201710933993A CN109627140A CN 109627140 A CN109627140 A CN 109627140A CN 201710933993 A CN201710933993 A CN 201710933993A CN 109627140 A CN109627140 A CN 109627140A
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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 a kind of mesitylene extraction and rectification separation methods.The method will reform C9 by de- light, Tuo Chonghou enriched mesitylene, and mesitylene is enriched to 60% content by 10% content at initial stage.Mesitylene pregnant solution and solvent are sent into extractive distillation column, extracting rectifying is carried out by extractant of glyceryl triacetate, extracting rectifying column overhead obtains the mesitylene that purity is 92% or more, 92% or more mesitylene passes through mesitylene treating column again, obtains the mesitylene that purity is 99.5% or more.The C9 component and solvent mixture that extracting rectifying and mesitylene are refining to obtain obtain solvent after C9 component and regeneration after solvent recovery tower separates, and regenerated solvent purity is 99%, can return to extractive distillation column reuse.The present invention isolates 99% or more mesitylene from reforming in C9, and mesitylene yield is not less than 90%；Mixed solvent is recycled simultaneously.
Description
Technical field
The present invention relates to a kind of production technologies that mesitylene is obtained from reformation carbon nine, and in particular to a kind of from catalysis weight
Whole C9 aromatic obtains mesitylene by the method for extracting rectifying.
Background technique
C9 aromatic hydrocarbons (C9A) is the significant by-products of petrochemical industry and coal coking device.Petroleum C9A is mainly from catalysis weight
The petrochemical plants such as whole, disproportionation, steam cracking and styrene.Wherein, catalytic reforming generates oil and isolates through extracting, rectifying
C9A accounts for 80% or more in remaining aromatic hydrocarbons after benzene, toluene and dimethylbenzene, although composition is more complicated, its component Relatively centralized.
Wherein n-proplbenzene, o-methylethylbenzene, p-methyl-ethylbenzene, the boiling point and mesitylene of pseudocumene are very close, with simple distillation
Method is difficult mesitylene from separating among them.
From the difficult point for reforming separating-purifying mesitylene in C9 aromatic hydrocarbons be how by it only poor 0.4 with mesitylene boiling point
DEG C o-methylethylbenzene separate.At present both at home and abroad production mesitylene more representational method have cryogenic crystallization method, extracting/
Isomerization process, transalkylation, reaction rectification method, extraction fractional distillation, pseudocumene isomerization-rectification method, alkylation-rectifying
Method, molecular sieve adsorption, Separation by Complexation method etc..In the production technology of all mesitylene, industrialization technology comparative maturity
It is that pseudocumene isomerization and alkylation-rectification method are these two types of.But alkylation process is by the material total overall reaction other than mesitylene
It generates high boiling substance and wastes useful resource.
Compared to other methods, extraction fractional distillation can realize being kept completely separate for mesitylene and the first and second benzene, and not will cause
The phenomenon that material other than mesitylene is wasted because of reaction has good industrial prospect.2004, Nanjing Normal University
The technique that a kind of rectifying combines separation C9A in extraction crossing is disclosed, using N- N-formyl morpholine N as extractant, tower top is distillated
In liquid, the content of mesitylene up to 98.5% or more, due to the solvent to the separative efficiency of mesitylene and o-methylethylbenzene compared with
Low, extractive distillation column number of theoretical plate N needs 123 pieces, and mesitylene yield is only 84%.2007, Beijing Chemical Research Institute with
Beijing Institute of Clothing Tech has developed a kind of method of double solvent extraction separation C9 aromatic cooperatively, i.e., using extracting rectifying and urgency essence
The separation integrated technology combined is evaporated, small-scale experiment result of study shows to be 102 pieces, reflux ratio 15, extract when number of theoretical plate
When agent/charging/urgency agent mass ratio is 7: 1: 0.3, the mesitylene product that purity is greater than 98.0% is can be obtained in tower top.Due to again
Introduce a kind of solvent, it is necessary to the solvent is separated and recycled, thus a urgency agent knockout tower need to be increased, the technology
Have the shortcomings that equipment one-time investment and process are relative complex.2013, Beijing Chemical Research Institute disclosed a kind of extraction essence
Double solvents of the fraction from mesitylene, mesitylene and o-methylethylbenzene relative volatility can be improved by 1.009 to 1.25, this is multiple
Bonding solvent is by N-Methyl pyrrolidone (93~99wt%) and alkali metal sulfates (1~7wt%, such as lithium sulfate, sodium sulphate or sulphur
Sour potassium) composition.Small-scale experiment the result shows that, when number of theoretical plate is 95 pieces, reflux ratio 4, solvent ratio are 4, tower top is available
The mesitylene product that yield is 98.1, purity is 98.6%.
Summary of the invention
The present invention status higher for mesitylene extracting rectifying number of theoretical plate, has invented a kind of new extractant, has answered
For in mesitylene extraction rectification technique, to reduce extracting rectifying number of theoretical plate, obtaining purity by extracting rectifying to be 99%
Mesitylene.This method simple process significantly reduces extracting rectifying column plate number compared with prior art, can obtain
The mesitylene resource in carbon nine is reformed in 99% or more mesitylene, effective use.
Technical solution proposed by the present invention are as follows: after reforming carbon nine by de- light, de- separation again, obtain mesitylene enrichment
Liquid.Mesitylene pregnant solution is sent into extractive distillation column, carry out extracting rectifying, extracting rectifying column overhead obtain purity be 95% with
On mesitylene, tower reactor obtains C9 component and extractant mixture.95% or more the mesitylene that tower top obtains is sent to equal
In trimethylbenzene treating column, the mesitylene that purity is 99% or more is obtained from mesitylene refined tower top, tower reactor obtains C9 group
Point and extractant mixture.C9 component and the extractant mixing that extractive distillation column tower reactor and mesitylene treating column tower reactor are obtained
Object is sent into extractant recovery tower, and after the separation of extractant recovery tower, extractant recycling column overhead obtains C9 component, and tower reactor obtains
The extractant that purity is 99% or more, extractant can return to extractive distillation column reuse.
Specifically, the present invention relates to the contents of following aspect:
In above-mentioned technical proposal, C9 to be separated generates oil from catalytic reforming unit, isolates through extracting, rectifying
C9A accounts for 80% or more in remaining aromatic hydrocarbons after benzene, toluene and dimethylbenzene.C9 is reformed by de- light removal light component, passes through de- weight
After isolating pseudocumene, mesitylene pregnant solution is obtained, mesitylene content is enriched to 60% left side by initial 10% or so
It is right.
In above-mentioned technical proposal, in mesitylene pregnant solution, mesitylene and o-methylethylbenzene are adopted since boiling point is close
It is separated with extraction rectifying method, extractant used is glyceryl triacetate.Glyceryl triacetate can be improved mesitylene with
Relative volatility between o-methylethylbenzene, to realize that isolated purity is 99% mesitylene
In above-mentioned technical proposal, the extractive distillation column, number of theoretical plate is 60~90 pieces, reflux ratio is 2~8, solvent
It is 3~10 than (the ratio between mixed solvent amount and inlet amount).After extracting rectifying, extracting rectifying column overhead mesitylene content reaches
93% or more, mesitylene yield is 92% or more.Extractive distillation column preferably number of theoretical plate is 60~80 pieces, reflux ratio 5
~6, solvent ratio is 3~5.
In above-mentioned technical proposal, the mesitylene treating column is vacuum rectification tower, and pressure is its reason of 5KPa~20KPa
It is 30~60 pieces by plate number, reflux ratio is 2~5, and after rectification under vacuum, the top of the distillation column produces 99% or more mesitylene,
The C9 component and solvent of tower reactor extraction C9 component and solvent and the extraction of extractive distillation column tower reactor enter jointly in extractant recovery tower.
In above-mentioned technical proposal, the extractant recovery tower is common rectifying tower, and number of theoretical plate is 30~60 pieces, reflux
Than being 2~5, after conventional distillation, the top of the distillation column produces C9 component, wherein extraction agent content, less than 1%, tower reactor extraction extracts
Agent, extraction agent content are greater than 99%, and extractant can be reentered in extractive distillation column and be reused.
Beneficial effect
Compared with the prior art, the advantages of the present invention are as follows can with the method for rectifying from reform C9 in isolate 99% with
On mesitylene, and mesitylene yield be not less than 90%, rectifying column number of theoretical plate is lower；Extractant is recycled simultaneously,
Environmentally harmful substance is not generated, realizes the effective use for reforming mesitylene resource in 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 reformation nine raw material group of carbon is smaller, and embodiment becomes representative with typical case's group and analyzed, heavy
The typical composition of whole carbon nine are as follows:
Embodiment 1
C9 is reformed by obtaining mesitylene pregnant solution, main component in mesitylene pregnant solution after de- light and de- weight are as follows:
P-methyl-ethylbenzene 0.28%, mesitylene 61.50%, o-methylethylbenzene 36.02%, pseudocumene 2.20%.
Mesitylene pregnant solution and solvent glyceryl triacetate are sent into extractive distillation column, extractive distillation column number of theoretical plate
It is 80, the charging of mesitylene pregnant solution is the 35th block of column plate, and solvent feed is the 4th block of column plate, reflux ratio 5, and solvent ratio is
3.Tower top obtains the mesitylene that purity is 93.2% after extracting rectifying, and mesitylene yield is 92.4%.By extracting rectifying
The mesitylene that obtained purity is 93.2% is sent into mesitylene treating column, and mesitylene treating column number of theoretical plate is 40
Block feeds as the 20th block of column plate, reflux ratio 3, and tower reactor pressure is 10KPa.After refining, mesitylene purity is 99.5%,
Yield is 98%.The tower reactor of extractive distillation column and mesitylene treating column is sent into solvent recovery tower, solvent recovery tower reason jointly
It is 40 pieces by plate number, feeds as the 20th block of column plate, reflux ratio 3.After refining, it is sweet that tower reactor produces the triacetic acid that purity is 99%
Grease, can be used as extractant reuse, and it is molten to can be used as carbon nine wherein extraction agent content is 0.04% for overhead extraction C9 component
Agent uses.
Embodiment 2
C9 is reformed by obtaining mesitylene pregnant solution, main component in mesitylene pregnant solution after de- light and de- weight are as follows:
P-methyl-ethylbenzene 0.28%, mesitylene 61.50%, o-methylethylbenzene 36.02%, pseudocumene 2.20%.
Mesitylene pregnant solution and solvent glyceryl triacetate are sent into extractive distillation column, extractive distillation column number of theoretical plate
It is 60, the charging of mesitylene pregnant solution is the 25th block of column plate, and solvent feed is the 4th block of column plate, reflux ratio 8, and solvent ratio is
10.Tower top obtains the mesitylene that purity is 93.8% after extracting rectifying, and mesitylene yield is 92.9%.By extracting rectifying
The mesitylene that obtained purity is 93.8% is sent into mesitylene treating column, and mesitylene treating column number of theoretical plate is 30
Block feeds as the 15th block of column plate, reflux ratio 5, and tower reactor pressure is 5KPa.After refining, mesitylene purity is 99.5%, is received
Rate is 98%.The tower reactor of extractive distillation column and mesitylene treating column is sent into solvent recovery tower jointly, solvent recovery tower is theoretical
Plate number is 30 pieces, is fed as the 15th block of column plate, reflux ratio 5.After refining, it is sweet that tower reactor produces the triacetic acid that purity is 99.3%
Grease, can be used as extractant reuse, and it is molten to can be used as carbon nine wherein extraction agent content is 0.04% for overhead extraction C9 component
Agent uses.
Embodiment 3
C9 is reformed by obtaining mesitylene pregnant solution, main component in mesitylene pregnant solution after de- light and de- weight are as follows:
P-methyl-ethylbenzene 0.28%, mesitylene 61.50%, o-methylethylbenzene 36.02%, pseudocumene 2.20%.
Mesitylene pregnant solution and solvent glyceryl triacetate are sent into extractive distillation column, extractive distillation column number of theoretical plate
It is 90, the charging of mesitylene pregnant solution is the 45th block of column plate, and solvent feed is the 4th block of column plate, reflux ratio 2, and solvent ratio is
2.Tower top obtains the mesitylene that purity is 92.4% after extracting rectifying, and mesitylene yield is 92%.Extracting rectifying is obtained
To purity be 92.4% mesitylene send into mesitylene treating column, mesitylene treating column number of theoretical plate be 60 pieces,
Charging is the 30th block of column plate, and reflux ratio 2, tower reactor pressure is 20KPa.After refining, mesitylene purity is 99.5%, yield
It is 98%.The tower reactor of extractive distillation column and mesitylene treating column is sent into solvent recovery tower, solvent recovery tower theoretical plate jointly
Number is 60 pieces, is fed as the 30th block of column plate, reflux ratio 2.After refining, tower reactor produces the triacetic acid glycerol that purity is 99%
Ester, can be used as extractant reuse, and overhead extraction C9 component can be used as nine solvent of carbon wherein extraction agent content is 0.04%
It uses.
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. a kind of mesitylene extraction and rectification separation method, it is characterised in that: after reforming C9 by de- light, de- separation again, obtain
Mesitylene pregnant solution send mesitylene pregnant solution into extractive distillation column, progress extracting rectifying, the extractive distillation column,
Its number of theoretical plate is 60~90 pieces, reflux ratio is 2~8, and extractant is glyceryl triacetate, extractant and mesitylene pregnant solution
Mass ratio be 3~10, extracting rectifying column overhead obtains mesitylene, and tower reactor obtains C9 component and extractant mixture, tower top
Obtained mesitylene is sent into mesitylene treating column, and tower reactor obtains C9 component and extractant mixture, by extractive distillation column
The C9 component and extractant mixture that tower reactor and mesitylene treating column tower reactor obtain are sent into extractant recovery tower, through extractant
After recovery tower separation, extractant recycling column overhead obtains C9 component, and the extractant that tower reactor obtains returns to extractive distillation column and repeats to make
With.
2. mesitylene extraction and rectification separation method according to claim 1, it is characterised in that: C9 to be separated is derived from
Catalytic reforming unit generates oil, after benzene, toluene and dimethylbenzene are isolated in extracting, rectifying in remaining aromatic hydrocarbons C9 account for 80% with
On.
3. mesitylene extraction and rectification separation method according to claim 1, it is characterised in that: the extractive distillation column
Number of theoretical plate be 60~80 pieces, reflux ratio is 5~6, and the mass ratio of extractant and mesitylene pregnant solution is 3~5.
4. mesitylene extraction and rectification separation method according to claim 1, it is characterised in that: the mesitylene purification
Tower is vacuum rectification tower, and pressure is 5KPa~20KPa, and number of theoretical plate is 30~60 pieces, and reflux ratio is 2~5, through decompression essence
After evaporating, the top of the distillation column produces mesitylene, and tower reactor produces C9 component and solvent.
5. mesitylene extraction and rectification separation method according to claim 1, it is characterised in that: the extractant recycling
Tower is common rectifying tower, and number of theoretical plate is 30~60 pieces, and reflux ratio is 2~5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202999A (en) * | 2020-02-10 | 2020-05-29 | 南京炼油厂有限责任公司 | Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene |
| CN112194553A (en) * | 2020-11-04 | 2021-01-08 | 成都宏鼎石化有限公司 | Method and device for separating carbon nonaarene mixture |
| CN114213208A (en) * | 2021-12-31 | 2022-03-22 | 黄河三角洲京博化工研究院有限公司 | Method for extracting, rectifying and purifying mesitylene by using efficient composite solvent |
| CN114292155A (en) * | 2021-12-31 | 2022-04-08 | 黄河三角洲京博化工研究院有限公司 | Method for thermally coupling and purifying mesitylene |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202999A (en) * | 2020-02-10 | 2020-05-29 | 南京炼油厂有限责任公司 | Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene |
| CN111202999B (en) * | 2020-02-10 | 2021-12-24 | 南京炼油厂有限责任公司 | Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene |
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| CN112194553B (en) * | 2020-11-04 | 2023-04-28 | 成都宏鼎石化有限公司 | Method and device for separating mixture of carbon nine aromatic hydrocarbon |
| CN114213208A (en) * | 2021-12-31 | 2022-03-22 | 黄河三角洲京博化工研究院有限公司 | Method for extracting, rectifying and purifying mesitylene by using efficient composite solvent |
| CN114292155A (en) * | 2021-12-31 | 2022-04-08 | 黄河三角洲京博化工研究院有限公司 | Method for thermally coupling and purifying mesitylene |
| CN114213208B (en) * | 2021-12-31 | 2024-01-30 | 黄河三角洲京博化工研究院有限公司 | Method for extracting, rectifying and purifying mesitylene by high-efficiency composite solvent |
| CN114292155B (en) * | 2021-12-31 | 2024-05-03 | 黄河三角洲京博化工研究院有限公司 | Method for purifying mesitylene through thermal coupling |
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Application publication date: 20190416 |