CN105985231A - Preparation of aromatic dicarboxylic acid - Google Patents
Preparation of aromatic dicarboxylic acid Download PDFInfo
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- CN105985231A CN105985231A CN201510079768.7A CN201510079768A CN105985231A CN 105985231 A CN105985231 A CN 105985231A CN 201510079768 A CN201510079768 A CN 201510079768A CN 105985231 A CN105985231 A CN 105985231A
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- distillating still
- organic solvent
- residual stream
- stripping tower
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/343—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas
- B01D3/346—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas the gas being used for removing vapours, e.g. transport gas
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
- C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/46—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention provides a method for removing residues from a first process stream comprising an organic solvent, water, a derivative of the organic solvent and the residues, comprising the steps of: i) feeding the first process stream to a solvent stripper comprising a still pot and a stripper column; ii) removing a vapour stream comprising the organic solvent, water and the derivative of the organic solvent from the stripper column; and iii) removing a residue stream from the still pot; characterised in that: the still pot and the stripper column form an integrated unit and the stripper column comprises a plurality of sieve trays. The present invention further provides an apparatus for carrying out the method.
Description
Technical field
The method and apparatus that the present invention relates to a kind of preparation for aromatic dicarboxylic acid.
Background technology
Aromatic dicarboxylic acid generally passes through the catalysis oxidation in organic solvent of hydrocarbon precursor and manufactures.Example is right
Phthalic acid (TA), it is widely used in prepares polyester, such as poly-(PETP) (PET).
It is referred to as " p-phthalic acid of purification " (PTA) as the TA needed for the reactant prepared for PET,
And usually contain the p-phthalic acid more than 99.97 weight %, preferably more than 99.99 weight %,
And less than 25ppm 4-carboxyl benzaldehyde (4-CBA).At industrial scale, be suitable in PET system
The PTA of standby middle use is generally prepared with two-phase method.First, by xylol at metallic catalyst
(such as, using air) is aoxidized to carry in the presence of (such as, cobalt and/or manganese salt or compound)
For " crude terephthalic acid " (CTA), as at such as US 2, described in 833,816.Then, will be logical
Cross CTA purification prepared by this oxidation reaction because its generally by impurity such as 4-CBA, to methylbenzene
Formic acid, and give the flaxen various foreign pigment of TA polluted.The purification of CTA is except needs
Outside at least one physical process (such as, crystallize, washing etc.), generally also need at least one and change
Learn and convert (such as, hydrogenation) to produce PTA.
PTA is generally viewed as batch item of merchandise, and its annual production has millions of tons, and therefore manufactures
Business expects to reduce its cost so that the economy prepared of PTA and efficiency maximize.This can be by reducing
Capital cost (such as, equipment cost) and variable cost are (such as, with waste treatment, starting material
Matter use, organic solvent, cost that heating fuel is relevant with deionized water) realize.
Therefore, it is intended that by design and production method to reclaim and recirculation organic solvent, thus by organic
The consumption of solvent (such as acetic acid) minimizes.It addition, along with organic solvent derivant such as methyl acetate
It is accumulate to steady-state level in the oxidation reaction, the organic solvent caused by being converted into these derivants
Consumption can by design described method thus also reclaim these derivants and they are recirculated back to
Oxidation reaction and minimize.Therefore, described method can be designed as reclaiming organic solvent, by organic molten
Agent is used for the task of washing its derivant to be reclaimed from expellant gas stream, and subsequently by derivant
It is recirculated back to oxidation reaction to realize above-mentioned two purpose.But, from some in this manufacture method
The organic solvent of stream (mother solution such as, the most first separated by CTA at CTA) comprises to be needed
The residue to remove it before this organic solvent can be used for washing task.Remove these residues
It is suitable to be probably because they are corrosive (such as hydrogen bromide) and/or because they comprise can
It is recovered and for valuable component (such as benzoic acid) elsewhere.
It is an object of the invention to provide a kind of for preparing the more economical and more effective of aromatic dicarboxylic acid
Method and apparatus.Further purpose will be clear to from description below.
Summary of the invention
A first aspect of the present invention provide a kind of for from comprising organic solvent, water, organic solvent spread out
The method of removal of residue in biological the first technique stream with residue, said method comprising the steps of:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower includes multiple
Sieve tray.
A first aspect of the present invention additionally provides a kind of solvent strippers, and described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower also includes many
Individual sieve tray.
A first aspect of the present invention additionally provides a kind of method of aromatic dicarboxylic acid for preparing purification,
Described method includes the catalysis oxidation in organic solvent of hydrocarbon precursor, said method comprising the steps of:
I) organic solvent aoxidizes hydrocarbon precursor in the presence of metallic catalyst to provide thick aromatics two
Carboxylic acid；And
II) thick aromatic dicarboxylic acid described in purification is to produce the aromatic dicarboxylic acid of purification,
Wherein said method is further comprising the steps of:
III) the first technique is flow to the solvent strippers expected to including distillating still and stripping tower, described
One technique stream comprises the organic solvent of method from the aromatic dicarboxylic acid for preparing purification, water, institute
State derivant and the residue of organic solvent；
IV) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from institute
State stripping tower to remove；And
V) residual stream is removed from described distillating still；
It is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower includes multiple
Sieve tray.
In a first aspect of the present invention, distillating still and stripping tower form integrated form unit, and i.e. they are not
It is by connecting the separate separate unit of pipeline, but is joined directly to each other.This structure need not with appointing
What pipeline connects distillating still and stripping tower, therefore reduces the capital cost of manufacture equipment.Inventor is
It was unexpectedly found that, relative to previous structure, as included the stripping tower of multiple baffle pan, make
The efficiency removing hydrogen bromide is improve so that move from stripping tower with the stripping tower including multiple sieve tray
Hydrogen bromide level in the steam stream removed reduces.Can be by the Part I of residual stream in residual stream
In using in reboiler loop, the heating of setting-out steam, then makes it via the first residual stream in distillating still
Entrance is back to distillating still.As used herein, " middle setting-out steam " finger pressure be about 5-10barA,
Or about 6-9barA or the saturated steam of about 8barA.Middle setting-out steam can be by with lower section
Formula obtains: the steam (such as " mesohigh steam (intermediate-pressure of higher pressure
Steam) ", finger pressure be about 10-50barA or about 12.5-40barA or about 15-35barA,
Or about 17.5-30barA or the saturated steam of about 20bar, or " high-pressure steam ", finger pressure
Power is about 50-150barA or about 75-125barA or the saturated steam of about 100barA)
Blood pressure lowering, and/or the flash distillation by the condensate to higher pressure and higher temperatures, and/or including hydrocarbon precursor
Producing in the method preparing aromatic dicarboxylic acid of catalysis oxidation in organic solvent, such as, pass through
The heat that the method produces is sent to current.
A second aspect of the present invention provides a kind of for from comprising organic solvent, water, described organic molten
The method removing described residue in the derivant of agent and the first technique stream of residue, described method bag
Include following steps:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that, described method is further comprising the steps of:
Iv) in using, setting-out steam heats the Part I of described residual stream；And
V) the described Part I making described residual stream is back to described distillating still.
A second aspect of the present invention additionally provides a kind of solvent strippers, and described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described solvent strippers also includes that residual stream reboiler loop, described residual stream reboiler are returned
Road is configured so that middle setting-out vapor source heats the residue removed from described first residual stream outlet
The Part I of stream, and make the described Part I of described residual stream via the in described distillating still
One residual stream entrance is back to described distillating still.
A second aspect of the present invention additionally provides a kind of method of aromatic dicarboxylic acid for preparing purification,
Described method includes the catalysis oxidation in organic solvent of hydrocarbon precursor, said method comprising the steps of:
I) in the presence of metallic catalyst, the hydrocarbon precursor in organic solvent is aoxidized to provide thick aromatics two
Carboxylic acid；And
II) thick aromatic dicarboxylic acid described in purification is to produce the aromatic dicarboxylic acid of purification,
Wherein said method is further comprising the steps of:
III) the first technique is flow to the solvent strippers expected to including distillating still and stripping tower, described
One technique stream comprises the organic solvent of method from the aromatic dicarboxylic acid for preparing purification, water, institute
State derivant and the residue of organic solvent；
IV) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from institute
State stripping tower to remove；And
V) residual stream is removed from described distillating still；
It is characterized in that, described method is further comprising the steps of:
VI) in using, setting-out steam heats the Part I of described residual stream；And
VII) the described Part I making described residual stream is back to distillating still.
Therefore, the Part I of heated residual stream is provided that present in evaporative distillation still any
Heat needed for the derivant of organic solvent, water and organic solvent.In using on loop of boiling again, setting-out steams
Gas rather than use Low pressure steam as previous structure (i.e. pressure is less than about the full of 5barA
And steam), it is allowed to use less heat exchanger for heat therefrom setting-out steam is sent to residue
The Part I of stream, therefore saves capital cost, reduces the cycle rate boiling in loop again, because of
This circulating pump allowing to use more low capacity, and reduce power consumption and the cost of circulating pump simultaneously
Both.Stripping tower can include multiple sieve tray.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the method and apparatus according to a first aspect of the present invention.
Fig. 2 is the schematic diagram of the method and apparatus according to a second aspect of the present invention.
Detailed description of the invention
This document describes multiple embodiments of the present invention.It should be appreciated that each embodiment middle finger
Fixed feature can be combined with other specific characteristics to provide other embodiments.
Should be appreciated that for preparing aromatic dicarboxylic acid by the catalysis oxidation in organic solvent of hydrocarbon precursor
The general operation of method and apparatus be well-known.Such as, as it has been described above, be suitable at PET
The p-phthalic acid (that is, the p-phthalic acid of purification) used in preparation is generally prepared with two-phase method.
First, by xylol in the existence of metallic catalyst (such as, cobalt and/or manganese salt or compound)
Lower oxidation (such as, using air) is to provide crude terephthalic acid.Then, will be anti-by this oxidation
The crude terephthalic acid purification that should prepare is with removal of impurity, such as 4-CBA and p-methylbenzoic acid, with
Generate the p-phthalic acid of purification.The purification of crude terephthalic acid is except at least one physical process of needs
Outside (such as, crystallize, washing etc.), generally also need at least one chemical conversion (such as, hydrogen
Change).
The preparation of aromatic dicarboxylic acid
The aromatic dicarboxylic acid prepared in the present invention be preferably selected from p-phthalic acid, phthalic acid and
Phthalic acid.Aromatic dicarboxylic acid is preferably p-phthalic acid.Therefore, residue generally comprises isophthalic two
Formic acid, phthalic acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzaldehyde, bromide (example
Such as hydrogen bromide), two or more mixture in catalytic component or these components.Residue also may be used
Comprise aromatic dicarboxylic acid itself.Hydrocarbon precursor is the compound of oxidable formation aromatic dicarboxylic acid.Therefore,
Hydrocarbon precursor is usually the position of the carboxylic acid substituent in required end product by such as C1-6Alkyl, first
Acyl group or the substituted benzene of acetyl group or naphthalene.Preferably hydrocarbon precursor is C1-6The substituted benzene of alkyl, specifically,
For xylol.Organic solvent is usually aliphatic carboxylic acid, such as acetic acid, or one or more these type of aliphatic series
Carboxylic acid and the mixture of water.The derivant of organic solvent is that the by-product as oxidation reaction is by organic molten
The compound that agent is formed.Such as, when organic solvent is acetic acid, the derivant of this organic solvent is permissible
For methyl acetate.Oxidation reaction can have wherein oxygen any under the conditions of carry out, such as, this reaction
Can carry out in atmosphere.Catalysts generally comprise the cobalt of soluble form and/or manganese (such as, it
Acetate), use bromine source (such as hydrogen bromide) as accelerator.The temperature of oxidation reaction is usual
In the range of about 100-250 DEG C, it is therefore preferable to about 150-220 DEG C.The pressure of any routine all may be used
For this reaction, suitably this reactant mixture is kept in the liquid state.
Oxidation panel performs to be catalyzed hydrocarbon precursor in organic solvent the function of oxidation, thus forms product stream
With discharge gas.Generally product stream is sent to crystallized region to form the first of thick aromatic dicarboxylic acid crystal
Serosity and overhead vapours.Generally the first serosity of thick aromatic dicarboxylic acid crystal is sent to segregation section, its
Middle mother solution is separated with thick aromatic dicarboxylic acid crystal, then can with liquid, aqueous mix to be formed thick
Second serosity of aromatic dicarboxylic acid crystal.Generally by this second serosity transmission of thick aromatic dicarboxylic acid crystal
To purifier apparatus, heat and hydrogenate, cooling down to be formed the aromatic dicarboxylic acid crystal of purification afterwards
Serosity.
In distilling period, the discharge gas of autoxidation section is separated to the liquid rich in organic solvent the most in the future
Body stream and rich in the steam stream of water.The liquid communication rich in organic solvent from distilling period often comprises
The organic solvent of 80-95% w/w, and generally return oxidation panel.From distilling period rich in
The steam flow of water often comprises the organic solvent of 0.1-5.0% w/w, and generally at condensation segment
Middle condensation is to form condensate flow and overhead gas.A part for condensate flow is typically used as being formed
The source of aqueous liquid of the second serosity of above-mentioned thick aromatic dicarboxylic acid crystal.A part for condensate flow is usual
Also form the scrub stream body source of the aromatic dicarboxylic acid crystal being used for the purification from purification devices.
Solvent strippers
Solvent strippers includes distillating still and stripping tower.This solvent strippers also includes for receiving first
First technique inflow entrance of technique stream.This entrance is usually located in distillating still, in order to by the first technique stream
Charging is to distillating still, but it may be alternatively located in stripping tower.Distillating still includes for removing first remaining
First residual stream outlet of logistics.This outlet is usually located in pedestal or the storage tank of distillating still, and
When deployed less than the liquid level in distillating still.Distillating still also includes air vent, and described air vent is used for will
Overhead vapours removes the first entrance to stripping tower.In a first aspect of the present invention, distillating still and
Stripping tower forms integrated form unit, and in this case, the air vent of distillating still is not by any centre
Pipeline but the first entrance of being directly joined in stripping tower.In a second aspect of the present invention, the most excellent
Choosing is distillating still and stripping tower formation integrated form unit.Stripping tower is generally of little more straight than distillating still
Footpath.Stripping tower also includes that air vent, described air vent are used for removing and comprises organic solvent, water and described
The steam stream of the derivant of organic solvent.Stripping tower is usually distillation column, and it includes that at least one is theoretical
Segregation section, it can be by tower tray, such as sieve tray, float valve tray or bubble cap tray, structured packing or carry
Other suitable structures for the surface of the quality transmission between gas phase and the liquid phase in tower provide.
In a first aspect of the present invention, stripping tower includes multiple sieve tray, and described sieve tray is reducing
The steam stream removed from stripping tower provides unexpected improvement in the level of hydrogen bromide.At this
In the second aspect of invention, accordingly it is also preferred that stripping tower includes multiple sieve tray.
In a second aspect of the present invention, solvent strippers also includes residual stream reboiler loop, its
It is configured to the Part I of the residual stream that heating removes from the first residual stream outlet, and makes described residual
The described Part I of excess stream is back to distillating still via the first residual stream entrance in distillating still.
In a first aspect of the present invention, accordingly it is also preferred that solvent strippers also includes residual stream reboiler
Loop, its Part I being configured to heat the residual stream removed from the first residual stream outlet, and
The described Part I making described residual stream returns via the first residual stream entrance in distillating still
To distillating still.First residual stream entrance is preferably placed on the liquid level in distillating still distillating still when deployed
The region of side.Therefore, the Part I of residual stream can experience sudden strain of a muscle in distillating still when it returns
Steam, the most described stream can evaporate and become the tower being sent to stripping tower from distillating still at least partially
A part for top steam.Therefore, reboiler loop improves in distillating still the concentration of residue in liquid,
And thus improve the concentration of residue in residual stream, i.e. reduce organic solvent in this liquid,
The concentration of the derivant of water and described organic solvent.In a second aspect of the present invention (and also, it is preferred that
Ground is in a first aspect of the present invention), use middle setting-out vapor source to realize heating, generally use heat exchange
Heat setting-out steam from this is sent to the Part I of residual stream by device (such as shell-and-tube heat exchanger).
As set forth above, it is possible to by the blood pressure lowering of the steam of higher pressure, and/or higher pressure and higher temperatures is cold
Setting-out steam in the flash distillation acquisition of condensate.It is alternatively possible to including that hydrocarbon precursor is in organic solvent
Being catalyzed setting-out steam in producing in the method being used for preparing aromatic dicarboxylic acid of oxidation, such as passing through should
The heat that method produces is sent to current.When heating residual stream, generally will therefrom setting-out steam produce
Raw middle pressure condensate feed is to relatively low setting-out vapour recovery system for future use.
Distillating still may also include residual stream recirculation circuit, its be configured to make residual stream second
Divide and be back to distillating still (such as by using pump) via the second residual stream entrance under stress.The
Two residual stream entrances are usually located in pedestal or the storage tank of distillating still, and when being preferably lower than use
Liquid level in distillating still.Therefore, the recirculation of residual stream can stir the liquid in distillating still so that
Need not mechanical agitator.
Solvent strippers may also include one or more two other technique inflow entrances to receive one or many
Individual other technique stream.Such as, solvent strippers can include that the second technique being positioned in distillating still flows into
Mouthful.This entrance can receive the second technique stream from air washer, for from its of this method
His the local steam stream produced removes the derivant of described organic solvent.Therefore, the second technique stream can
For comprising the washed liquid stream of water and organic solvent, by described organic solvent in air washer
Derivant remove from this liquid stream.Alternately, or additionally, solvent strippers can include being positioned at gas
In stripper, such as, it is positioned at the 3rd technique inflow entrance at the top of stripping tower.This entrance can receive the 3rd
Technique stream, this stream can comprise organic solvent, water and the derivant of described organic solvent.This 3rd work
Skill stream can be used as the wash fluid of the overhead vapours removed from distillating still.
First technique stream
First technique stream comprises organic solvent, water, the derivant of described organic solvent and residue.The
One technique stream be preferably from include hydrocarbon precursor in organic solvent catalysis oxidation for preparing
The stream of the method for aromatic dicarboxylic acid (such as TA).Specifically, the first technique stream is preferably therefrom
Separated go out aromatic dicarboxylic acid crystal mother solution.More specifically, the first technique stream has been preferably the most
Isolate the mother solution (i.e. mother solution derives from as above " the first serosity ") of thick aromatic dicarboxylic acid crystal.
Process further
The Part III of residual stream can be fed to residue vaporizer with in evaporation residue logistics
In any one of the derivant of remaining water, organic solvent and/or described organic solvent at least one
Point.It is then possible to quencher process the molten residue stream of gained to separate and to reclaim its various components,
As described in co-pending Patent application GB 1414292.1, this full patent texts is by drawing
With being combined in this.Steam flow from residue vaporizer often comprises organic solvent and water, and should
Steam stream can be back to solvent strippers from residue vaporizer, is generally back to distillating still.
Organic solvent, water and the derivant of described organic solvent can be comprised by remove from stripping tower
Steam be streamed to air-lift device for from the derivant of organic solvent described in this steaming air flow recovery, from
And the organic solvent stream of purification is provided, the derivant of organic solvent described in described organic solvent stream
Mass concentration reduces relative to the mass concentration of the derivant of the described organic solvent in steam stream.
The present invention will be further described with reference to the drawings.
Fig. 1 is the signal of the method and apparatus of preferred embodiment according to the first aspect of the invention
Figure.Feeding the first technique stream 10a to solvent strippers 10, this first technique stream comprises organic molten
Agent (preferably acetic acid), water, the derivant (preferably methyl acetate) of organic solvent and residue are (excellent
Select M-phthalic acid, phthalic acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzaldehyde, bromine
Compound and the mixture of catalytic component).Solvent strippers 10 is by distillating still 20 and stripping tower 30
Composition, the two forms integrated form unit.With comprising the derivative of organic solvent, water and described organic solvent
The stream 10b of thing washs the overhead vapours removed from distillating still 20 in stripping tower 30.From stripping tower
30 remove steam stream 10c, and this steam stream comprises organic solvent, water and the derivant of described organic solvent.
Removal of residue stream 10d from distillating still 20.By the Part I transmission of residual stream 10d
To the first pump 40 and by residual stream 40a charging to heat exchanger 60, provide pressure to this heat exchanger
It is about middle setting-out vapor feed 60a of 8barA.Condensate flow 60b is removed also from heat exchanger 60
Fed to relatively low pressure steam recovery system for future use.By heated residual stream 60c
Feed to distillating still 20 via the entrance of ullage in distillating still 20.Residual stream 40b is fed
To residue vaporizer 70.The stream 70a of organic solvent and water will be comprised via liquid level in distillating still 20
The entrance of top feeds to distillating still 20.By melted residual stream 70b from residue vaporizer 70
Remove, for being processed further.The Part II of residual stream 10d is sent to the second pump 50.
Residual stream 50a is back to distillating still 20 via the entrance below liquid level in distillating still 20.
Fig. 2 is the signal of the method and apparatus of the preferred embodiment according to a second aspect of the present invention
Figure.Feeding the first technique stream 110a to solvent strippers 110, this first technique stream comprises organic
Solvent (preferably acetic acid), water, the derivant (preferably methyl acetate) of described organic solvent and remnants
Thing (preferably M-phthalic acid, phthalic acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzene first
The mixture of aldehyde, bromide and catalytic component).Solvent strippers 110 is gentle by distillating still 120
Stripper 130 forms.Vapor stream of top of the tower 120a is removed from distillating still 120 via air vent, and will
Its charging is to the entrance of stripping tower 130, in porch with comprising organic solvent, water and described organic molten
The stream 110b of the derivant of agent washs this vapor stream of top of the tower.By liquid stream 130b from stripping tower 130
(although drawing respectively, but stream 120a and 120b is permissible to remove and feed the entrance to distillating still 120
Delivered by single pipeline or pipeline).Steam stream 110c is removed, this steam stream from stripping tower 130
Comprise organic solvent, water and the derivant of described organic solvent.
Residual stream 110d is removed from distillating still 120.The Part I of residual stream 110d is passed
Delivering to the first pump 140 and feed residual stream 140a to heat exchanger 160, this heat exchanger provides
Pressure is had to be about middle setting-out vapor feed 160a of 8barA.By condensate flow 160b from heat exchanger
160 remove and fed to relatively low pressure steam recovery system for future use.By heated residual
Excess stream 160c feeds to distillating still 120 via the entrance of ullage in distillating still 120.By residual
Excess stream 140b feeds to residue vaporizer 170.The stream 170a warp of organic solvent and water will be comprised
Fed to distillating still 120 by the entrance of ullage in distillating still 120.By melted residual stream
170b removes from residue vaporizer 170, for being processed further.By residual stream 110d
Part II is sent to the second pump 150.Residual stream 150a via liquid level in distillating still 120 below
Entrance be back to distillating still 120.
Embodiment according to the disclosure, it is provided that below scheme.
Scheme 1
A kind of for from comprising the of organic solvent, water, the derivant of described organic solvent and residue
The method removing described residue in one technique stream, said method comprising the steps of:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower includes multiple
Sieve tray.
Scheme 2
According to the method described in scheme 1, described method is further comprising the steps of:
Iv) in using, setting-out steam heats the Part I of described residual stream；And
V) the described Part I making described residual stream is back to described distillating still.
Scheme 3
A kind of for from comprising the of organic solvent, water, the derivant of described organic solvent and residue
The method removing described residue in one technique stream, said method comprising the steps of:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that, described method is further comprising the steps of:
Iv) in using, setting-out steam heats the Part I of described residual stream；And
V) the described Part I making described residual stream is back to described distillating still.
Scheme 4
According to the method described in scheme 3, wherein said stripping tower includes multiple sieve tray.
Scheme 5
According to the method described in any one in scheme 2-4, wherein in step v), described residue
The described Part I of stream experiences flash distillation in described distillating still.
Scheme 6
According to the method described in any one in scheme 2-5, it is right that wherein said middle setting-out steam derives from
The blood pressure lowering of the steam of higher pressure, and/or to higher pressure and the flash distillation of the condensate of higher temperatures and/or
Generating in the method prepare aromatic dicarboxylic acid, the described method for preparing aromatic dicarboxylic acid includes
The catalysis oxidation in described organic solvent of the hydrocarbon precursor.
Scheme 7
According to the method described in any one in front scheme, wherein said first technique stream is for using by oneself
Stream in the method preparing aromatic dicarboxylic acid, the described method for preparing aromatic dicarboxylic acid includes hydrocarbon
Precursor catalysis oxidation in described organic solvent.
Scheme 8
According to the method described in scheme 7, wherein said first technique stream for the most separated go out thick aromatics
The mother solution of dicarboxylic acid crystals.
Scheme 9
According to the method described in scheme 7 or scheme 8, wherein said aromatic dicarboxylic acid is p-phthalic acid.
Scheme 10
According to the method described in scheme 9, wherein said residue includes M-phthalic acid, O-phthalic
Acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzaldehyde, bromide, catalytic component or they
Mixture.
Scheme 11
According to the method described in any one in front scheme, wherein said organic solvent is acetic acid.
Scheme 12
According to the method described in scheme 11, the derivant of wherein said organic solvent is methyl acetate.
Scheme 13
According to the method described in any one in front scheme, wherein flow to described first technique to expect to
Described distillating still in step i).
Scheme 14
According to the method described in any one in front scheme, described method is further comprising the steps of:
Vi) make the Part II of described residual stream under stress via the liquid being positioned in described distillating still
One or more entrances under face are back to described distillating still.
Scheme 15
According to the method described in any one in front scheme, described method is further comprising the steps of:
Vii) Part III of described residual stream is fed to residue vaporizer；And
Viii) stream comprising described organic solvent and water is made to be back to described steaming from described residue vaporizer
Evaporate still.
Scheme 16
According to the method described in any one in front scheme, described method is further comprising the steps of:
Ix) by described steaming gas stream to being used for spreading out from organic solvent described in described organic solvent air stripping
Biological air-lift device.
Scheme 17
A kind of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower also includes many
Individual sieve tray.
Scheme 18
According to the solvent strippers described in scheme 17, wherein said distillating still also includes residual stream again
Boiling device loop, described residual stream reboiler loop configuration heats from described for setting-out vapor source in using
The Part I of the residual stream that the first residual stream outlet removes, and make the described of described residual stream
Part I is back to described distillating still via the first residual stream entrance.
Scheme 19
A kind of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described solvent strippers also includes that residual stream reboiler loop, described residual stream reboiler are returned
Road is configured so that middle setting-out vapor source heats the residue removed from described first residual stream outlet
The Part I of stream, and make the described Part I of described residual stream via the in described distillating still
One residual stream entrance is back to described distillating still.
Scheme 20
According to the solvent strippers described in scheme 19, wherein said stripping tower includes multiple sieve tray.
Scheme 21
According to the solvent strippers described in any one in scheme 17-20, wherein said solvent strippers
Also include that residual stream recirculation circuit, described residual stream recirculation circuit are configured to make described remnants
The Part II of logistics is back to described distillation via the second residual stream entrance in described distillating still
Still.
Additionally, in some embodiments, the disclosure also includes following additional aspects.
Additional aspects 1
A kind of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Remove the air vent of overhead vapours,
Stripping tower, described stripping tower includes:
Receive the first entrance of described overhead vapours；And
Remove the air vent of steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and
Described distillating still and described stripping tower form integrated form unit, and described stripping tower also includes many
Individual sieve tray.
Additional aspects 2
According to the solvent strippers described in additional aspects 1, wherein said distillating still is pressed in also including using
The Part I of the residual stream that source of water vapor heating removes from described first residual stream outlet, and make
The described Part I of described residual stream is back to described distillating still via the first residual stream entrance
Residual stream reboiler loop.
Additional aspects 3
A kind of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Remove the air vent of overhead vapours,
Stripping tower, described stripping tower includes:
Receive the first entrance of described overhead vapours；And
Remove the air vent of steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and
During described solvent strippers also includes using, setting-out vapor source heats from described first residual stream
The Part I of residual stream that outlet removes, and make the described Part I of described residual stream via
The first residual stream entrance in described distillating still is back to the residual stream reboiler of described distillating still
Loop.
Additional aspects 4
According to the solvent strippers described in additional aspects 3, wherein said distillating still and described air stripping turriform
Become integrated form unit.
Additional aspects 5
According to the solvent strippers described in additional aspects 3 or additional aspects 4, wherein said distillation column is
Including the distillation column of at least one theoretical separation stages, described theoretical distillation tray by tower tray, regular fill out
Other of the surface of the quality transmission between material or offer gas phase and liquid phase in tower are suitably tied
Structure provides.
Additional aspects 6
According to the solvent strippers described in additional aspects 5, wherein said tower tray is sieve tray, float valve
Tower tray or bubble cap tray.
Additional aspects 7
According to the solvent strippers described in additional aspects 6, wherein said stripping tower includes multiple sieve-plate tower
Dish.
Additional aspects 8
According to the solvent strippers described in any one in additional aspects 1-7, wherein said solvent air stripping
Device also includes that the Part II making described residual stream is via the second residual stream in described distillating still
Entrance is back to the residual stream recirculation circuit of described distillating still.
Additional aspects 9
According to the solvent strippers described in additional aspects 8, wherein said second residual stream entrance is positioned at
In the pedestal of described distillating still or storage tank.
Additional aspects 10
According to the solvent strippers described in additional aspects 8, wherein said second residual stream entrance is less than
Liquid level in distillating still during use.
Claims (21)
1. one kind is used for from comprising organic solvent, water, the derivant of described organic solvent and residue
The first technique stream in remove the method for described residue, said method comprising the steps of:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower includes multiple
Sieve tray.
Method the most according to claim 1, described method is further comprising the steps of:
Iv) in using, setting-out steam heats the Part I of described residual stream；And
V) the described Part I making described residual stream is back to described distillating still.
3. one kind is used for from comprising organic solvent, water, the derivant of described organic solvent and residue
The first technique stream in remove the method for described residue, said method comprising the steps of:
I) described first technique is flow to the solvent strippers expected to including distillating still and stripping tower；
Ii) the steam stream of the derivant of described organic solvent, water and described organic solvent will be comprised from described
Stripping tower removes；And
Iii) residual stream is removed from described distillating still；
It is characterized in that, described method is further comprising the steps of:
Iv) in using, setting-out steam heats the Part I of described residual stream；And
V) the described Part I making described residual stream is back to described distillating still.
Method the most according to claim 3, wherein said stripping tower includes multiple sieve tray.
5. according to the method described in any one in claim 2-4, wherein in step v), described
The described Part I of residual stream experiences flash distillation in described distillating still.
6., according to the method described in any one in claim 2-5, wherein said middle setting-out steam comes
Come from the blood pressure lowering of the steam to higher pressure, and/or to higher pressure and the flash distillation of the condensate of higher temperatures
And/or generate in the method for preparing aromatic dicarboxylic acid, described for preparing aromatic dicarboxylic acid
Method includes the catalysis oxidation in described organic solvent of the hydrocarbon precursor.
7. according to the method described in any one in front claim, wherein said first technique stream
For from the stream in the method for preparing aromatic dicarboxylic acid, the described side for preparing aromatic dicarboxylic acid
Method includes the catalysis oxidation in described organic solvent of the hydrocarbon precursor.
Method the most according to claim 7, wherein said first technique stream is the most separated
Go out the mother solution of thick aromatic dicarboxylic acid crystal.
9. according to the method described in claim 7 or claim 8, wherein said aromatic dicarboxylic acid
For p-phthalic acid.
Method the most according to claim 9, wherein said residue include M-phthalic acid,
Phthalic acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzaldehyde, bromide, catalyst group
Point or their mixture.
11. according to the method described in any one in front claim, and wherein said organic solvent is
Acetic acid.
12. methods according to claim 11, the derivant of wherein said organic solvent is second
Acid methyl ester.
13. according to the method described in any one in front claim, wherein by described first technique
Flow to the described distillating still expected to step i).
14. according to the method described in any one in front claim, and described method also includes following
Step:
Vi) make the Part II of described residual stream under stress via the liquid being positioned in described distillating still
One or more entrances under face are back to described distillating still.
15. according to the method described in any one in front claim, and described method also includes following
Step:
Vii) Part III of described residual stream is fed to residue vaporizer；And
Viii) stream comprising described organic solvent and water is made to be back to described steaming from described residue vaporizer
Evaporate still.
16. according to the method described in any one in front claim, and described method also includes following
Step:
Ix) by described steaming gas stream to being used for spreading out from organic solvent described in described organic solvent air stripping
Biological air-lift device.
17. 1 kinds of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described distillating still and described stripping tower form integrated form unit, and described stripping tower also includes many
Individual sieve tray.
18. solvent strippers according to claim 17, wherein said distillating still also includes residual
Excess stream reboiler loop, described residual stream reboiler loop configuration adds for setting-out vapor source in using
The Part I of the residual stream that heat removes from described first residual stream outlet, and make described residue
The described Part I of stream is back to described distillating still via the first residual stream entrance.
19. 1 kinds of solvent strippers, described solvent strippers includes:
Distillating still, described distillating still includes:
First residual stream outlet；And
Air vent, described air vent is used for removing overhead vapours,
Stripping tower, described stripping tower includes:
First entrance, described first entrance is used for receiving described overhead vapours；And
Air vent, described air vent is used for removing steam stream,
Wherein said solvent strippers also includes the first technique inflow entrance, and it is characterized in that:
Described solvent strippers also includes that residual stream reboiler loop, described residual stream reboiler are returned
Road is configured so that middle setting-out vapor source heats the residue removed from described first residual stream outlet
The Part I of stream, and make the described Part I of described residual stream via the in described distillating still
One residual stream entrance is back to described distillating still.
20. solvent strippers according to claim 19, wherein said stripping tower includes multiple
Sieve tray.
21. according to the solvent strippers described in any one in claim 17-20, wherein said molten
Agent air stripper also includes that residual stream recirculation circuit, described residual stream recirculation circuit are configured to make
The Part II of described residual stream is back to via the second residual stream entrance in described distillating still
Described distillating still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110803618.1A CN113527084A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GBGB1417621.8A GB201417621D0 (en) | 2014-10-06 | 2014-10-06 | Production of an aromatic dicarboxylic acid |
| GB1417621.8 | 2014-10-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110803618.1A Division CN113527084A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
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| CN105985231A true CN105985231A (en) | 2016-10-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510079768.7A Pending CN105985231A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acid |
| CN201520108187.7U Active CN204637616U (en) | 2014-10-06 | 2015-02-13 | Solvent strippers |
| CN202110803618.1A Pending CN113527084A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
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| CN201520108187.7U Active CN204637616U (en) | 2014-10-06 | 2015-02-13 | Solvent strippers |
| CN202110803618.1A Pending CN113527084A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
Country Status (3)
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|---|---|
| CN (3) | CN105985231A (en) |
| GB (1) | GB201417621D0 (en) |
| WO (1) | WO2016055463A1 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751015A (en) * | 2003-02-21 | 2006-03-22 | 三菱化学株式会社 | Method for producing aromatic carboxylic acid |
| EP2569584A2 (en) * | 2010-05-10 | 2013-03-20 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Method and apparatus for separating air by cryogenic distillation |
| CN103245130A (en) * | 2012-02-14 | 2013-08-14 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling heat and water in dried tail gas by heat pump working media and device of method |
| CN102224132B (en) * | 2008-10-02 | 2013-09-11 | 陶氏环球技术有限责任公司 | Apparatus, systems, and methods for purification of isocyanate mixtures |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2580951A1 (en) * | 1996-02-09 | 1997-08-14 | Invista Technologies S.A.R.L. | Azeotropic distillation process |
| US7048835B2 (en) * | 2002-02-12 | 2006-05-23 | Amt International, Inc. | System and method for acetic acid recovery during terephthalic acid production |
| KR100733400B1 (en) * | 2005-08-01 | 2007-06-29 | 아신기술 주식회사 | Azeotropic Distillation Process for Separating Acetic Acid, Methyl Acetate and Water |
| CN103012102B (en) * | 2011-09-27 | 2014-09-17 | 中国石油化工股份有限公司 | Method of recovering acetic acid and water in production of aromatic carboxylic acid |
-
2014
- 2014-10-06 GB GBGB1417621.8A patent/GB201417621D0/en not_active Ceased
-
2015
- 2015-02-13 CN CN201510079768.7A patent/CN105985231A/en active Pending
- 2015-02-13 CN CN201520108187.7U patent/CN204637616U/en active Active
- 2015-02-13 CN CN202110803618.1A patent/CN113527084A/en active Pending
- 2015-10-06 WO PCT/EP2015/073028 patent/WO2016055463A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751015A (en) * | 2003-02-21 | 2006-03-22 | 三菱化学株式会社 | Method for producing aromatic carboxylic acid |
| CN102224132B (en) * | 2008-10-02 | 2013-09-11 | 陶氏环球技术有限责任公司 | Apparatus, systems, and methods for purification of isocyanate mixtures |
| EP2569584A2 (en) * | 2010-05-10 | 2013-03-20 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Method and apparatus for separating air by cryogenic distillation |
| CN103245130A (en) * | 2012-02-14 | 2013-08-14 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling heat and water in dried tail gas by heat pump working media and device of method |
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| Publication number | Publication date |
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| GB201417621D0 (en) | 2014-11-19 |
| CN204637616U (en) | 2015-09-16 |
| WO2016055463A1 (en) | 2016-04-14 |
| CN113527084A (en) | 2021-10-22 |
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