CN105837394A - Purifying method of highly-pure 1,2,3-trimethylbenzene - Google Patents
Purifying method of highly-pure 1,2,3-trimethylbenzene Download PDFInfo
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- CN105837394A CN105837394A CN201610209495.8A CN201610209495A CN105837394A CN 105837394 A CN105837394 A CN 105837394A CN 201610209495 A CN201610209495 A CN 201610209495A CN 105837394 A CN105837394 A CN 105837394A
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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
- 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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Abstract
The invention provides a purifying method of highly-pure 1,2,3-trimethylbenzene. The method comprises a raw material preprocessing process and an extraction and rectification process, and adopts integrated differential thermal coupling design. The tower top of a preliminary heavy component removal tower T2 supplies heat to the top bottom of a preliminary light component removal tower T1, the tower top of an extraction and rectification tower T3 supplies heat to the tower bottom of the preliminary heavy component removal tower T2, the tower top of a solvent recovery tower T4 supplies heat to the tower bottom of the extraction and rectification tower T3, and steam supplies heat to the solvent recovery tower T4; and the preliminary light component removal tower T1, the preliminary heavy component removal tower T2 and the extraction and rectification tower T3 are respectively provided with reboilers. Sulfolane/dimethyl sulfoxide with the mass ratio of 10-5:1 is adopted as an extractant, and the integrated differential thermal coupling extraction and rectification design is adopted, so the device investment and the operating cost are reduced, and the yield of 1,2,3-trimethylbenzene is improved. A system in the invention allows highly-pure 1,2,3-trimethylbenzene to be effectively extracted from mixed C9 aromatic hydrocarbon solvent oil, the purity of the above product to be not smaller than 99wt% and the yield to be 92-95%.
Description
Technical field
The present invention relates to the method for purification of a kind of high-purity Hemimellitene, particularly relate to a kind of from mixing C9Aromatic solvent naphtha carries
The method of pure Hemimellitene.
Background technology
Hemimellitene is as a kind of important medicine, chemical industry intermediate, and it is producing aniline dyes, benzene-1,2,3-tricarboxylic acid,
Synthesis musk tibetene, produces the pharmaceutical preparations tools such as platelet anticoagulant and has been widely used.Mixing C9Aromatic hydrocarbons is essentially from refining
Oil factory reformer, a large amount of Hemimellitenes wherein contained blend component as gasoline mostly is burned off, and the wasting of resources is tight
Weight.Use rational isolation technics to obtain highly purified Hemimellitene product, its processing and utilization had great significance,
And huge economical, societal benefits can be created.It separates difficult point and essentially consists in the components such as Hemimellitene and indane at present
Boiling point difference the least, use conventional distillation be difficult to obtain high-purity Hemimellitene product.
Application for a patent for invention publication number CN 1900034 A is " from mixing C9The method purifying Hemimellitene in aromatic solvent naphtha "
Use alkylation transformation approach separating-purifying Hemimellitene.Utilize the method can obtain the Hemimellitene of mass fraction more than 92%
Product, but this method complex technical process, less economical, catalyst life is short, is not easy to industrialized production.
Application for a patent for invention publication number CN 101704706 A " from heavy aromatics separating-purifying Hemimellitene and the side of indane
Method " utilize adsorbing separation to combine precise distillation method to obtain mass fraction and be not less than the Hemimellitene product of 95%, but the method
Process is loaded down with trivial details, and catalyst activity is low, the life-span is short, and cost is high, industrialized production difficulty.
It is therefore proposed that a kind of product purity is high, process energy consumption is little, and operating procedure is simple, it is easy to industrialized Hemimellitene
Process for separating and purifying is necessary.
Summary of the invention
It is an object of the invention to provide a kind of from mixing C9Aromatic solvent naphtha obtains the production method of high-purity Hemimellitene,
Sulfolane/dimethyl sulfoxide that process uses mass ratio to be 10～5:1 makees extractant, uses integrated differential pressure heat coupling extraction
Distillation design, reduces equipment investment and running cost, improves the yield of Hemimellitene simultaneously.This system can effectively from
Mixing C9Extracting high-purity Hemimellitene in aromatic solvent naphtha, make product purity >=99wt%, yield is between 92～95%.
The technical solution of the present invention is as follows:
The method of purification of a kind of high-purity Hemimellitene, including pretreatment of raw material and extracting rectifying two parts, uses process integration
Differential pressure heat Coupling Design.
Described integrated differential pressure heat Coupling Design flow process is: pre-weight-removing column tower top is pre-lightness-removing column tower bottom heating, extractive distillation column
Tower top is pre-weight-removing column tower bottom heating, and solvent recovery column overhead is extractive distillation column tower bottom heating, solvent recovery tower steam
Heat supply；Pre-lightness-removing column, pre-weight-removing column and extractive distillation column are provided with reboiler.
Raw material pretreatment portion includes pre-lightness-removing column and pre-weight-removing column, and extracting rectifying part includes that extractive distillation column and solvent return
Receive tower；Pre-lightness-removing column removes in raw material more low-boiling component than Hemimellitene；The group that the removing of pre-weight-removing column is higher than indane boiling point
Point；Extractive distillation column increases Hemimellitene and the relative volatility of indane, removes indane, obtains Hemimellitene product；Molten
Agent recovery tower reclaims extractant.
Operational approach is: mixing C to be purified9Raw material enters the middle part of pre-lightness-removing column, sloughs most light component and damages
Losing a small amount of Hemimellitene, pre-lightness-removing column reboiler utilizes pre-weight-removing column top gaseous phase logistics condensation as thermal source, takes off through pre-
Overhead condensation liquid after light tower reboiler heat exchange returns to pre-weight-removing column part as backflow, part extraction；Pre-lightness-removing column tower reactor
C is mixed after taking off gently9Logistics enters the middle part of pre-weight-removing column, sloughs most heavy constituent and loses a small amount of Hemimellitene,
Pre-weight-removing column reboiler utilizes extractive distillation column top gaseous phase logistics to condense as thermal source, after pre-weight-removing column reboiler heat exchange
Overhead condensation liquid return to extracting rectifying tower section as backflow, part extraction；The Hemimellitene that pre-weight-removing column tower top concentrates
Logistics enters in the middle part of extractive distillation column, and circulating solvent logistics adds on extractive distillation column top, removes indane through extracting rectifying,
Extracting rectifying column overhead obtains high-purity Hemimellitene product, and extractive distillation column reboiler utilizes solvent recovery tower top gaseous phase thing
Stream condensation is as thermal source, and the overhead condensation liquid after extractive distillation column reboiler heat exchange returns to solvent recovery tower section as returning
Stream, part extraction；The heavy constituent logistics such as extractant and indane enters solvent recovery tower, and solvent recovery column overhead obtains indane
And heavy constituent, the extractant being recycled at the bottom of tower；The extractant reclaimed returns extraction after mixing with the fresh extractant supplemented
Rectifying column.
Described pre-lightness-removing column tower top operation pressure 5～30KPa, tower reactor operation temperature 80～140 DEG C, number of theoretical plate 30～150,
Feed entrance point is theoretical plate 10～70, reflux ratio 20～70.
Described pre-weight-removing column tower top operation pressure 20～90KPa, tower reactor operation temperature 120～190 DEG C, number of theoretical plate 40～150,
Feed entrance point is theoretical plate 20～80, reflux ratio 4～40.
Described extracting rectifying column overhead operation pressure 70～100KPa, bottom temperature 220～280 DEG C, number of theoretical plate 100～200,
Feedstock position is theoretical plate 40～120, and extractant feed position is theoretical plate 5～30, solvent ratio 5～15, reflux ratio
3～12.
Described solvent recovery column overhead operation pressure 70～100KPa, bottom temperature 260～300 DEG C, number of theoretical plate 30～100,
Feed entrance point is theoretical plate 8～32, reflux ratio 5～20.
The present invention, by system carries out step rectification of reducing pressure, reduces mixing C9Mixture in aromatic solvent naphtha material liquid
Boiling point, increases the relative volatility between each component, reduces separating difficulty, improve product yield；Process uses
Differential pressure heat coupling rectification also reduces the energy consumption of process.The accurate pressure reduction thermal coupling extracting rectifying of the present invention is relative to traditional
Rectification separating technology, process total energy consumption reduces about 30～50%.
The invention have the advantage that
(1) present invention uses the design of accurate pressure reduction thermal coupling extracting rectifying, by decompression step rectification reduce separating difficulty and
Energy consumption.
(2) present invention proposes a kind of novel extraction rectification technique, uses novel sulfolane/dimethyl sulfoxide (mass ratio
10～5:1) doing mixed extractant, can improve the purity (>=99wt%) of Hemimellitene further, decompression operation is further
Improve the yield (between 92～95%) of Hemimellitene.
(3) present invention uses Precision Integrated pressure reduction thermal coupling step reduced pressure distillation process, energy consumption can be greatly lowered, relatively pass
System rectification process saving energy 30～50%.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of a kind of high-purity Hemimellitene method of purification of the present invention.
Wherein:
Illustrate: the pre-lightness-removing column of T1；The pre-weight-removing column of T2；T3 extractive distillation column；T4 solvent recovery tower；E1 is pre-de-light
Tower reboiler；E2 pre-weight-removing column reboiler；E3 extractive distillation column reboiler；1 mixing C to be purified9Raw material；2 take off
The light component stream removed；3 de-light after mix C9Logistics；4 pre-weight-removing column top gaseous phase logistics；5 through pre-lightness-removing column again
Overhead condensation liquid after boiling device heat exchange；The 6 Hemimellitene logistics concentrated；The heavy constituent logistics of 7 removings；8 extracting rectifyings
Column overhead gaseous stream；The 9 overhead condensation liquid after pre-weight-removing column reboiler heat exchange；10 circulating solvent logistics；11 is high
Pure Hemimellitene product；The heavy constituent logistics such as 12 extractants and indane；13 solvent recovery tower top gaseous phase logistics；14 warps
Overhead condensation liquid after extractive distillation column reboiler heat exchange；15 indanes and heavy constituent logistics；16 extractants reclaimed；17
The fresh extractant supplemented.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.
A kind of from mixing C9Aromatic solvent naphtha extracts the flow process of high-purity Hemimellitene, including pretreatment of raw material and extracting rectifying
Two parts, relate to pre-lightness-removing column T1, pre-weight-removing column T2, extractive distillation column T3 and solvent recovery tower T4.Wherein raw material is pre-
Process part includes pre-lightness-removing column T1 and pre-weight-removing column T2, and extracting rectifying part includes extractive distillation column T3 and solvent recovery
Tower T4.The purpose of pre-lightness-removing column T1 is more low-boiling component than Hemimellitene in removing raw material；The purpose of pre-weight-removing column T2
It is to remove the component higher than indane boiling point；The purpose of extractive distillation column T3 is increase Hemimellitene and indane relatively volatile
Degree, removes indane, obtains Hemimellitene product；The purpose of solvent recovery tower T4 is to reclaim extractant.
Assembly of the invention is as shown in Figure 1:
Mixing C to be purified9The feeding line of raw material 1 is connected in the middle part of pre-lightness-removing column T1, the light component stream 2 of removing
Pipeline be connected with pre-lightness-removing column T1 tower top, de-light after mix C9The pipeline of logistics 3 is connected in the middle part of pre-weight-removing column T2,
Pre-lightness-removing column T1 tower reactor arranges pre-lightness-removing column reboiler E1；The pipeline of pre-weight-removing column top gaseous phase logistics 4 and pre-lightness-removing column
Reboiler E1 is connected, the pipeline of the overhead condensation liquid 5 after pre-lightness-removing column reboiler heat exchange and pre-weight-removing column T2 tower top
Being connected, the pipeline of Hemimellitene logistics 6 concentrated through pre-weight-removing column T2 is connected with extractive distillation column T3, pre-de-weight
Tower T2 tower reactor connects the pipeline of the heavy constituent logistics 7 of removing, and pre-weight-removing column T2 tower reactor arranges pre-weight-removing column reboiler E2；
The pipeline of extractive distillation column top gaseous phase logistics 8 is connected with pre-weight-removing column reboiler E2, changes through pre-weight-removing column reboiler
The pipeline of the overhead condensation liquid 9 after heat is connected with extractive distillation column T3 top, the pipeline of circulating solvent logistics 10 and extraction
Taking rectifying column T3 top to be connected, extractive distillation column T3 tower top connects the pipeline of high-purity Hemimellitene product 11, extraction
The pipeline of the heavy constituent logistics such as agent and indane 12 is connected with solvent recovery tower T4, and extractive distillation column T3 tower reactor arranges extraction
Take rectifying column reboiler E3；The pipeline of solvent recovery tower top gaseous phase logistics 13 is connected with extractive distillation column reboiler E3,
The pipeline of the overhead condensation liquid 14 after extractive distillation column reboiler heat exchange is connected with solvent recovery tower T4 top, indane
And the pipeline of heavy constituent logistics 15 is connected with solvent recovery tower T4 tower top, the pipeline of the extractant 16 of recovery returns with solvent
Receive tower T4 tower reactor to be connected.
Whole flow process uses process integration precision pressure reduction thermal coupling design, i.e. high-pressure tower tower top to boil to the offer of lower pressure column tower reactor again
Heat, not only reduces the energy consumption of process but also saves equipment investment, reduce to greatest extent whole flow process equipment investment and
Operating cost.
Pre-weight-removing column T2 tower top is pre-lightness-removing column T1 tower bottom heating, and extractive distillation column T3 tower top is at the bottom of pre-weight-removing column T2 tower
Heat supply, solvent recovery tower T4 tower top is extractive distillation column T3 tower bottom heating, solvent recovery tower T4 steam heating.
Material flow is as follows:
Mixing C to be purified9Raw material 1 enters the middle part of pre-lightness-removing column T1, sloughs most light component and loses a small amount of
Hemimellitene (logistics 2), pre-lightness-removing column reboiler E1 utilizes pre-weight-removing column top gaseous phase logistics 4 to condense as thermal source,
Overhead condensation liquid 5 after pre-lightness-removing column reboiler heat exchange returns to pre-weight-removing column T2 part as backflow, part extraction；
Pre-lightness-removing column T1 tower reactor mixes C after taking off gently9Logistics 3 enters the middle part of pre-weight-removing column T2, sloughs most heavy constituent also
Losing a small amount of Hemimellitene (logistics 7), pre-weight-removing column reboiler E2 utilizes extractive distillation column top gaseous phase logistics 8 cold
Solidifying as thermal source, the overhead condensation liquid 9 after pre-weight-removing column reboiler heat exchange returns to extractive distillation column T3 part as returning
Stream, part extraction；The Hemimellitene logistics 6 that pre-weight-removing column T2 tower top concentrates enters in the middle part of extractive distillation column T3, circulation
Solvent stream 10 adds on extractive distillation column T3 top, removes indane through extracting rectifying, and extractive distillation column T3 tower top obtains
To high-purity Hemimellitene product (logistics 11), extractive distillation column reboiler E3 utilizes solvent recovery tower top gaseous phase logistics
13 condensations are as thermal source, and the overhead condensation liquid 14 after extractive distillation column reboiler heat exchange returns to solvent recovery tower T4 part
As backflow, part extraction；The heavy constituent logistics such as extractant and indane 12 enters solvent recovery tower T4, solvent recovery tower
T4 tower top obtains indane and heavy constituent (logistics 15), and the extractant being recycled at the bottom of tower (logistics 16) also returns extraction essence
Evaporating tower T3, supplementary fresh extractant is realized by logistics 17.
The present invention, in order to preferably mate the heat between each tower, controls pre-lightness-removing column T1 tower top operation pressure 5～30KPa,
Tower reactor operation temperature 80～140 DEG C, number of theoretical plate 30～150, feed entrance point 10～70 (theoretical plate), reflux ratio 20～70；
Pre-weight-removing column T2 tower top operation pressure 20～90KPa, tower reactor operation temperature 120～190 DEG C, number of theoretical plate 40～150, enters
Material position 20～80 (theoretical plate), reflux ratio 4～40；Extractive distillation column T3 tower top operation pressure 70～100KPa, tower reactor
Temperature 220～280 DEG C, number of theoretical plate 100～200, feedstock position 40～120 (theoretical plate), extractant feed position
Put 5～30 (theoretical plates), solvent ratio 5～15, reflux ratio 3～12；Solvent recovery tower T4 tower top operation pressure 70～100KPa,
Bottom temperature 260～300 DEG C, number of theoretical plate 30～100, feed entrance point 8～32 (theoretical plate), reflux ratio 5～20.
Embodiment one:
Feedstock amount is 1000kg/h, and sulfolane/dimethyl sulfoxide mass ratio is 10:1, and feed composition is as shown in the table:
Process conditions are as follows:
The Hemimellitene product purity produced under above-mentioned process conditions is 99.2%, and product recovery rate is: 93.9%.
Embodiment two:
Feedstock amount is 1200kg/h, and sulfolane/dimethyl sulfoxide mass ratio is 8:1, and feed composition is as shown in the table:
Process conditions are as follows:
The Hemimellitene product purity produced under above-mentioned process conditions is 99.3%, and product recovery rate is: 94.4%.
Embodiment three:
Feedstock amount is 1200kg/h, and sulfolane/dimethyl sulfoxide mass ratio is 5:1, and feed composition is as shown in the table:
Process conditions are as follows:
The Hemimellitene product purity produced under above-mentioned process conditions is 99.5%, and product recovery rate is: 92.8%.
The method of purification of a kind of high-purity Hemimellitene of present invention disclosure and proposition, those skilled in the art can be by using for reference this
Literary composition content, suitably changes the links such as condition route and realizes, although the method for the present invention and technology of preparing are by preferably implementing
Example is described, and person skilled substantially can be to described herein in without departing from present invention, spirit and scope
Method and technology path be modified or reconfigure, realize final technology of preparing.Special needs to be pointed out is,
All similar replacements and change apparent to those skilled in the art, they are considered as being included in this
In spirit, scope and content.
Claims (9)
1. the method for purification of a high-purity Hemimellitene, it is characterised in that: include pretreatment of raw material and extracting rectifying two parts, adopt
By process integration differential pressure heat Coupling Design.
Method the most according to claim 1, it is characterised in that integrated differential pressure heat Coupling Design flow process is: pre-weight-removing column tower top is
Pre-lightness-removing column tower bottom heating, extracting rectifying column overhead is pre-weight-removing column tower bottom heating, and solvent recovery column overhead is extractive distillation column tower
End heat supply, solvent recovery tower steam heating；Pre-lightness-removing column, pre-weight-removing column and extractive distillation column are provided with reboiler.
Method the most according to claim 1 or claim 2, it is characterised in that raw material pretreatment portion includes pre-lightness-removing column and pre-weight-removing column,
Extracting rectifying part includes extractive distillation column and solvent recovery tower；Pre-lightness-removing column removes in raw material more low-boiling component than Hemimellitene；
The component that the removing of pre-weight-removing column is higher than indane boiling point；Extractive distillation column increases Hemimellitene and the relative volatility of indane, removes indenes
Full, obtain Hemimellitene product；Solvent recovery tower reclaims extractant.
Method the most according to claim 3, it is characterised in that mixing C to be purified9Raw material enters the middle part of pre-lightness-removing column,
Sloughing most light component and lose a small amount of Hemimellitene, pre-lightness-removing column reboiler utilizes pre-weight-removing column top gaseous phase logistics cold
Solidifying as thermal source, the overhead condensation liquid after pre-lightness-removing column reboiler heat exchange returns to pre-weight-removing column part as backflow, part extraction；
Pre-lightness-removing column tower reactor mixes C after taking off gently9Logistics enters the middle part of pre-weight-removing column, sloughs most heavy constituent and loses a small amount of company
Trimethylbenzene, pre-weight-removing column reboiler utilizes extractive distillation column top gaseous phase logistics to condense as thermal source, changes through pre-weight-removing column reboiler
Overhead condensation liquid after heat returns to extracting rectifying tower section as backflow, part extraction；The Hemimellitene that pre-weight-removing column tower top concentrates
Logistics enters in the middle part of extractive distillation column, and circulating solvent logistics adds on extractive distillation column top, removes indane, extraction through extracting rectifying
Taking rectifying column tower top and obtain high-purity Hemimellitene product, extractive distillation column reboiler utilizes solvent recovery tower top gaseous phase logistics to condense
As thermal source, the overhead condensation liquid after extractive distillation column reboiler heat exchange returns to solvent recovery tower section and adopts as backflow, part
Go out；The heavy constituent logistics such as extractant and indane enters solvent recovery tower, and solvent recovery column overhead obtains indane and heavy constituent, at the bottom of tower
The extractant being recycled；The extractant reclaimed returns extractive distillation column after mixing with the fresh extractant supplemented.
The most according to claim 4 from method, it is characterised in that: pre-lightness-removing column tower top operation pressure 5～30KPa, tower reactor is grasped
Making temperature 80～140 DEG C, number of theoretical plate 30～150, feed entrance point is theoretical plate 10～70, reflux ratio 20～70.
The most according to claim 4 from method, it is characterised in that: pre-weight-removing column tower top operation pressure 20～90KPa, tower reactor is grasped
Making temperature 120～190 DEG C, number of theoretical plate 40～150, feed entrance point is theoretical plate 20～80, reflux ratio 4～40.
The most according to claim 4 from method, it is characterised in that: extracting rectifying column overhead operation pressure 70～100KPa, tower
Still temperature 220～280 DEG C, number of theoretical plate 100～200, feedstock position is theoretical plate 40～120, and extractant feed position is
Theoretical plate 5～30, solvent ratio 5～15, reflux ratio 3～12.
The most according to claim 4 from method, it is characterised in that: solvent recovery column overhead operation pressure 70～100KPa, tower
Still temperature 260～300 DEG C, number of theoretical plate 30～100, feed entrance point is theoretical plate 8～32, reflux ratio 5～20.
The most according to claim 4 from method, it is characterised in that: the extractant selected by extracting rectifying part is mass ratio 10～5:1
Sulfolane/dimethyl sulfoxide.
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| 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 |
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