CN204637629U - For reclaiming the equipment of derivative of organic solvent and the equipment for the preparation of aromatic dicarboxylic acid from the first process flow - Google Patents

For reclaiming the equipment of derivative of organic solvent and the equipment for the preparation of aromatic dicarboxylic acid from the first process flow Download PDF

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CN204637629U
CN204637629U CN201520107979.2U CN201520107979U CN204637629U CN 204637629 U CN204637629 U CN 204637629U CN 201520107979 U CN201520107979 U CN 201520107979U CN 204637629 U CN204637629 U CN 204637629U
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organic solvent
equipment
derivative
storage
stream
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克里斯托弗·霍华德·杰克逊
伊恩·詹姆斯·奥尔森·罗伯茨
安东尼·彼得·约翰·林巴赫
阿努伊·古普塔
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Koch Technology Solutions UK Ltd
Invista North America LLC
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Invista Technologies SARL Switzerland
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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
    • 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
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • 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
    • B01D3/38—Steam distillation
    • 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
    • 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
    • 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
    • C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • 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)

Abstract

The disclosure provides a kind of equipment of the derivative for reclaiming organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, described equipment comprises: air-lift device, and described air-lift device comprises: stripping tower; The storage tank of liquid is received from described stripping tower; The condenser of overhead streams is received from described stripping tower; And the first process flow entrance; Wherein said storage tank comprises weir plate in the perpendicular that is separated with the storage of the organic solvent of pollution by the storage of the organic solvent of purifying; Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And the organic solvent flow export of the purifying that the organic solvent stream of purifying removed from the storage of the organic solvent of described purifying.

Description

For reclaiming the equipment of derivative of organic solvent and the equipment for the preparation of aromatic dicarboxylic acid from the first process flow
Technical field
The disclosure relates to a kind of equipment and one group of equipment for the preparation of aromatic dicarboxylic acid of the derivative for reclaiming organic solvent from the first process flow.
Background technology
Aromatic dicarboxylic acid is usually by the catalytic oxidation preparation in organic solvent of hydrocarbon precursor.Example is terephthalic acid (TPA) (TA), and it is widely used in prepares polyester, as poly-(PETP) (PET).Be called as " terephthalic acid (TPA) of purifying " (PTA) as the TA needed for the reactant prepared for PET, and usually containing the terephthalic acid (TPA) more than 99.97 % by weight, preferably more than 99.99 % by weight, and be less than 25ppm 4-carboxyl benzaldehyde (4-CBA).At industrial scale, the PTA being suitable for using in PET manufactures is prepared with two-stage process usually.First, by paraxylene, under the existence of metallic catalyst (such as, cobalt and/or manganese salt or compound), oxidation is (such as, use air) to provide " crude terephthalic acid " (CTA), as at such as US 2,833, described in 816.Then, by the CTA purifying prepared by this oxidation reaction because its usually by impurity as 4-CBA, p-methylbenzoic acid, and give TA flaxen various foreign pigment and polluted.The purifying of CTA, outside at least one physical process of needs (such as, crystallization, washing etc.), also needs at least one chemical conversion (such as, hydrogenation) to produce PTA usually.
PTA is regarded as batch item of merchandise usually, and its annual production has millions of tons, and therefore manufacturer expects to reduce its cost with the economy making PTA manufacture and maximizing efficiency.This is by reducing capital cost (such as, equipment cost) and variable cost (such as, to waste treatment, initial substance uses, organic solvent, heating fuel and deionized water are relevant cost) realizes.
Therefore, expect by design and production method to reclaim and to recycle the consumption that organic solvent minimizes organic solvent (such as, acetic acid).WO 96/06065 describes the azeotropic distillation of the acetic acid of the vapor stream of top of the tower to the oxidation reaction from manufacture TA.Use entrainer if isobutyl acetate or n-propyl acetate are to promote water removing from acetic acid.Top product from distillation is sent to independent condenser.The condensate separation of gained is become organic phase and aqueous phase, and wherein said organic phase is back to distillation, and reclaims entrainer to be recycled to distillation from described aqueous phase, and reclaims methyl acetate for subsequent treatment.
Because the derivative of organic solvent such as methyl acetate is accumulate to steady-state level in the oxidation reaction, so by being also reclaim these derivatives and they are recycled to oxidation reaction can minimize organic solvent by its consumption to the conversion of these derivatives by described method design.Therefore, by described method design for reclaiming organic solvent, this organic solvent can be used to reclaim its derivative from effluent gas flow when the task of washing, being recirculated to oxidation reaction subsequently, to realize above-mentioned two objects.
Object of the present disclosure is to provide a kind of for the manufacture of the more economical of aromatic dicarboxylic acid and more effective method and apparatus.Further object will be obvious from following description.
Utility model content
The disclosure provides a kind of equipment of the derivative for reclaiming organic solvent from the first process flow, and described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
The disclosure also provides a kind of equipment of the derivative for reclaiming organic solvent from the first process flow, and described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Receive the air-lift device of the first process flow, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower, and
Prepare the oxidation reactor of aromatic dicarboxylic acid,
Wherein, described equipment also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
The disclosure also provides a kind of equipment for the preparation of aromatic dicarboxylic acid, and described equipment comprises
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow from the first crystallizer or the second crystallizer, the equipment of the described derivative from the first process flow recovery organic solvent from the first crystallizer or the second crystallizer comprises
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
The disclosure also provides a kind of equipment for the preparation of aromatic dicarboxylic acid, and described equipment comprises
Prepare the oxidation reactor of aromatic dicarboxylic acid;
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow, the described equipment reclaiming the derivative of organic solvent from the first process flow comprises:
Receive the air-lift device of the first process flow, and described air-lift device comprises
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower,
The wherein said equipment reclaiming the derivative of organic solvent from the first process flow also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
In addition, present disclose provides a kind of for the method from the derivative for the preparation of the first process flow recovery organic solvent in the method for aromatic dicarboxylic acid, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, the described method for the preparation of aromatic dicarboxylic acid comprises the catalytic oxidation of hydrocarbon precursor in described organic solvent in oxidation reactor, and the method for the derivative of described recovery organic solvent comprises the following steps
I) described first process flow is fed to air-lift device, described air-lift device comprises stripping tower and storage tank;
Ii) the organic solvent stream of purifying is removed from described storage tank; And
Iii) overhead streams is sent to condenser from described stripping tower,
Wherein, step I i) in the purifying removed from described storage tank organic solvent stream the mass concentration of derivative of described organic solvent lower than step I) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device, and, optionally
Wherein, step I ii) in the mass concentration being sent to the derivative of the described organic solvent in the overhead streams of described condenser be greater than step I) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device.
The disclosure additionally provides a kind of equipment of the derivative for reclaiming organic solvent from the first process flow, and described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device is configured to reception first process flow, and described air-lift device comprises:
Stripping tower;
Storage tank, described storage tank is arranged as and receives liquid from described stripping tower; With
Condenser, described condenser is arranged as and receives overhead streams from described stripping tower, and
Oxidation reactor, described oxidation reactor is used for the preparation of aromatic dicarboxylic acid, and the preparation of described aromatic dicarboxylic acid comprises the catalytic oxidation of hydrocarbon precursor in described organic solvent,
Wherein, described equipment also comprises:
Be sent to the device of described oxidation reactor from described condenser for the stream of the derivative by comprising described organic solvent.
Stripping tower and storage tank form integrated form unit usually, that is, they are not the separate units be separated by connecting pipeline structure, but directly engage each other.Preferably, stripping tower, storage tank and condenser form integrated form unit.These configurations eliminate connection storage tank and stripping tower, and the needs of any pipeline configuration of stripping tower and condenser, and because this reducing the capital cost of manufacturing installation.
Preferably, method of the present disclosure also comprises and will comprise following steps: the liquid stream of the derivative of described organic solvent is fed to described oxidation reactor from the upper area of described condenser or described stripping tower.As mentioned above, reclaim the derivative of organic solvent by this way and be recirculated to oxidation reactor and contribute to minimizing machine solvent by being converted into the loss of this derivative.
Preferably, the disclosure also comprises and the organic solvent stream of described purifying is fed to cleaning section, to be removed from gaseous flow by the derivative of described organic solvent.In washing task, use the organic solvent stream of purifying (corresponding to and still unpurified organic solvent stream) to add the recovery of derivative from gaseous flow of organic solvent.In addition, because the amount of the derivative of organic solvent described in the organic solvent stream of purifying reduces, the derivative of organic solvent by the derivative of described organic solvent from the loss reduction caused by the evaporation of the organic solvent stream of purifying.Further preferably first the organic solvent stream of purifying is cooled, then be fed to cleaning section.Which in turns increases the recovery of derivative from gaseous flow of described organic solvent.
Accompanying drawing explanation
Fig. 1 is the schematic diagram according to method and apparatus of the present disclosure.
Detailed description of the invention
This document describes multiple embodiment of the present disclosure.Will be appreciated that, the feature of specifying in each embodiment can be combined to provide other embodiments with other specific characteristics.
Should be appreciated that the general operation for being prepared the method and apparatus of aromatic dicarboxylic acid by hydrocarbon precursor catalytic oxidation is in organic solvent well-known.Such as, as mentioned above, the terephthalic acid (TPA) (that is, the terephthalic acid (TPA) of purifying) being suitable for using in PET preparation is prepared with two-stage process usually.First, by paraxylene under the existence of metallic catalyst (such as, cobalt and/or manganese salt or compound) oxidation (such as, in atmosphere) to provide crude terephthalic acid.Then, by the crude terephthalic acid purifying prepared by this oxidation reaction to remove impurity, as 4-CBA and p-methylbenzoic acid, to produce the terephthalic acid (TPA) of purifying.The purifying of crude terephthalic acid, outside at least one physical process of needs (such as, crystallization, washing etc.), also needs at least one chemical conversion (such as, hydrogenation) usually.
The preparation of aromatic dicarboxylic acid
The aromatic dicarboxylic acid prepared in the disclosure can be selected from terephthalic acid (TPA), phthalic acid and M-phthalic acid.Aromatic dicarboxylic acid is preferably terephthalic acid (TPA).Hydrocarbon precursor is the compound of oxidable formation aromatic dicarboxylic acid.Therefore, hydrocarbon precursor is generally the position quilt of the carboxylic acid substituent in required end product as C 1-6the benzene that alkyl, formoxyl or acetyl group replace or naphthalene.Preferred hydrocarbon precursor is C 1-6the benzene that alkyl replaces particularly, is paraxylene.Organic solvent is generally aliphatic carboxylic acid, as acetic acid, or the mixture of one or more these type of aliphatic carboxylic acids and water.The derivative of organic solvent is the compound formed by described organic solvent as the accessory substance of oxidation reaction.Such as, when organic solvent is acetic acid, the derivative of this organic solvent can be methyl acetate.Oxidation reaction is carried out under can having any condition of oxygen wherein, and such as, this reaction can be carried out in atmosphere.Catalysts comprises cobalt and/or the manganese (such as, their acetate) of soluble form usually, uses bromine source (as hydrogen bromide) as promoter.The temperature of oxidation reaction, usually in the scope of about 100-250 DEG C, is preferably about 150-220 DEG C.The pressure of any routine all can be used for this reaction, suitably to be kept in the liquid state by this reactant mixture.
The oxidation panel generally including oxidation reactor performs the function of hydrocarbon precursor catalytic oxidation in organic solvent, thus forms product stream and emission gases.Product stream is sent to the crystallized region usually at least comprising the first crystallizer and the second crystallizer usually, to form the first slurries and the overhead vapours of thick aromatic dicarboxylic acid crystal.Usually the first slurries of thick aromatic dicarboxylic acid crystal are sent to segregation section, wherein mother liquor and thick aromatic dicarboxylic acid crystal are separated, then can mix with liquid, aqueous the second slurries forming thick aromatic dicarboxylic acid crystal.Usually the second slurries of this thick aromatic dicarboxylic acid crystal are sent to purification devices, heat and carry out hydrogenation, cooling the slurries of the aromatic dicarboxylic acid crystal forming purifying afterwards.
In distilling period, usually in the future the emission gases of autoxidation section is separated to the liquid stream that is rich in organic solvent and is rich in the steam stream of water.The liquid stream being rich in organic solvent from distilling period comprises the organic solvent of 80-95% w/w usually, and usually returns oxidation panel.The steam flow being rich in water from distilling period often comprises the organic solvent of 0.1-5.0% w/w, and usually in condensation segment condensation to form condensate flow and overhead gas.A part for condensate flow is typically used as the source of aqueous liquid of the second slurries for the formation of above-mentioned thick aromatic dicarboxylic acid crystal.A part for condensate flow also forms the scrub stream body source be used for from the aromatic dicarboxylic acid crystal of the purifying of purification devices usually.
Air-lift device
Air-lift device comprises stripping tower and storage tank, and it is set to collect from the liquid bottom stripping tower.Stripping tower is generally the destilling tower comprising at least one theoretical separation stages, and it can be provided by other suitable structures on the surface of tower tray (as sieve tray, float valve tray or bubble cap tray), structured packing or the quality transmission between the gas phase be provided in tower and liquid phase.
Storage tank can comprise weir plate in the perpendicular that is separated with the storage of the organic solvent of pollution for the storage of the organic solvent by purifying.Therefore, when air-lift device in use time, the storage of the organic solvent of purifying contains the organic solvent of purifying, and the storage of organic solvent polluted contains the organic solvent of pollution.As used herein, " organic solvent of purifying " refers to body or the stream of the liquid of the organic solvent that the mass concentration of the derivative comprising wherein organic solvent reduces relative to the mass concentration of the derivative of organic solvent in the first process flow.Usually, at least 50 quality %, at least 60 quality % of the organic solvent stream of purifying, at least 70 quality %, at least 80 quality % or at least 90 quality % are organic solvents, and being less than 5 quality % or being less than 2 quality % or being less than 1 quality % or being less than 0.5 quality % or being less than 0.2 quality % or being less than the derivative that 0.1 quality % is organic solvent of the organic solvent stream of purifying.The surplus normally water of the organic solvent stream of purifying, although the impurity (such as, organic impurities) that may there is trace (such as, being less than 1 quality % separately).As used herein, " organic solvent of pollution " refers to that the mass concentration of the derivative of wherein organic solvent is greater than body or the stream of the liquid of the mass concentration of the derivative of the organic solvent in the organic solvent of purifying.As used herein, " mass concentration " refers to the mark that the quality (or mass velocity) of given component is shared in the quality (or mass velocity) of given fluid bulk (or stream).Particularly, in the organic solvent polluted, mass concentration and the ratio of the mass concentration of the derivative of organic solvent in the organic solvent of purifying of the derivative of organic solvent can be greater than 1: 1 or be more than or equal to 2: 1 or be more than or equal to 3: 1 or be more than or equal to 4: 1 or be more than or equal to 5: 1 or be more than or equal to 6: 1 or be more than or equal to about 7: 1 or be more than or equal to about 8: 1 or be more than or equal to about 9: 1 or be more than or equal to about 10: 1, and can be less than or equal to about 50: 1 or be less than or equal to about 100: 1.As used herein, " perpendicular " means weir plate to be orientated to and the storage being arranged on two organic solvents of sump bottom is separated by effectively; Weir plate does not need and horizontal plane (such as, it may become the angle between 70 ° and 110 ° with horizontal plane, or becomes the angle between 80 ° and 100 ° with horizontal plane, or with the angle of horizontal plane into about 90 °).The air-lift device organic solvent of purifying can be overflowed across storage that weir plate enters the organic solvent of pollution can be operated, the storage of organic solvent polluted is diluted effectively by the adding of organic solvent of purifying (that is, in the storage of the organic solvent of pollution, the mass concentration of the derivative of organic solvent declines).The organic solvent stream of purifying can remove from storage tank via the outlet be communicated with the storage fluid of the organic solvent of pollution with the storage of the organic solvent of purifying respectively with the organic solvent stream of pollution.Therefore, for removing the outlet of the organic solvent stream of purifying and the bottom of the storage of the storage of the organic solvent of purifying and the organic solvent of pollution can being arranged in for the outlet of the organic solvent stream removing pollution.These streams can use in the other places of the method subsequently.Particularly, usually the organic solvent stream of purifying is under high pressure sent to cleaning section or oxidation reactor.The more high position that the organic solvent polluted usually under low pressure is sent to other tasks or is recycled in air-lift device.
As mentioned above, stripping tower and storage tank form integrated form unit usually.Therefore, the liquid from stripping tower falls in storage tank in the situation not through any intermediate conduit structure.Storage tank also can comprise the deflector being arranged such that the storage being imported into the organic solvent of purifying from the liquid of stripping tower.Therefore, deflector can be arranged in the top of the storage of the organic solvent of pollution and at angle, make the liquid fallen on deflector fall into the storage of the organic solvent of purifying subsequently.
First process flow is directed to stripping tower usually, the derivative of organic solvent is separated from organic solvent self by this stripping tower, thus overhead streams and tower bottom flow (the organic solvent stream of purifying) are provided, in overhead streams, the mass concentration of the derivative of organic solvent increases relative to the mass concentration of the derivative of organic solvent in the first process flow, and in tower bottom flow, the mass concentration of the derivative of organic solvent declines relative to the mass concentration of the derivative of organic solvent in the first process flow.But, can by the first process flow guiding to storage tank higher than the At The Height of liquid level in storage tank, this causes the first process flow part flash distillation usually, thus generates the steam entered bottom stripping tower.
Air-lift device can comprise the one or more entrances for receiving one or more process flow.Such as, first condensate flow that the condensation from the vapor stream of top of the tower from the first crystallizer can be obtained is fed to the first condensate flow entrance.First condensate flow entrance can be arranged in storage tank, makes the liquid coming from the first condensate flow enter the storage of the organic solvent of pollution.In addition, second condensate flow that the condensation from the vapor stream of top of the tower from the second crystallizer can be obtained is fed to the second condensate flow entrance.Second condensate flow entrance can be arranged in storage tank, makes the liquid coming from the second condensate flow enter the storage of the organic solvent of pollution.One or both in first and second condensate flow entrances can be arranged in above the storage of the organic solvent of baffle plate (if existence) below and pollution.Therefore, the storage of the organic solvent of pollution can substitute the solvent barrel of the stream of the organic solvent for collecting pollution, thus reduces the capital cost of the method further.(namely the organic solvent of pollution can be flowed through external fluid passage, this fluid passage is arranged in air-lift device outside) higher point (that is, being fed to the entrance of air-lift device) of air-lift device is fed to from the storage of organic solvent polluted.Particularly, the stream of the organic solvent of pollution can be fed to stripping tower (that is, being fed to the entrance in stripping tower) from the storage of the organic solvent polluted.The stream of clean organic solvent can be fed to the storage (that is, being fed in the storage of the organic solvent of purifying or the entrance of top) of the organic solvent of purifying.
Overhead streams from stripping tower is transferred into condenser.As mentioned above, stripping tower, storage tank and condenser preferably form integrated form unit, to avoid the needs for any intermediate conduit structure linked together by each unit.Therefore, the steam from stripping tower rises in condenser when not passing any intermediate conduit structure.Similarly, condenser can be designed so that the condensate of condenser can drop to stripping tower.Condenser has cold water charging to supply with the condensation at least partially of the volatile component by steam usually, thus forms liquid stream and the steam stream of the derivative of the organic solvent comprised from the first process flow air lift.The upper area (such as, top tray from stripping tower) of liquid stream from condenser or stripping tower can be taken out, then be fed to oxidation reactor, with the recirculation of the derivative to oxidation reactor that realize organic solvent.Liquid stream can flow with other (such as, the one or more tower bottom flows from cleaning section) merges, and/or processed in its path to oxidation reactor.Alternatively, liquid stream can be fed directly to oxidation reactor, that is, its path to oxidation reactor form to change it without undergoing any intermediate treatment.
Because main purpose of the present disclosure reclaims the derivative of organic solvent, instead of water is separated from organic solvent, therefore the disclosure does not preferably adopt entrainer in air-lift device.Specifically, the disclosure does not preferably adopt isobutyl acetate, n-propyl acetate or the boiling point entrainer between isobutyl acetate and the boiling point of n-propyl acetate in air-lift device.
Cleaning section
The derivative of organic solvent can remove from gaseous flow by cleaning section.As used herein, " removing " refers to that specified ingredients is from specifying partially or completely removing of stream.Therefore, 10 quality % of specified ingredients or 20 quality % or 30 quality % or 40 quality % or 50 quality % or 60 quality % or 70 quality % or 80 quality % or 90 quality % or 95 quality % or 99 quality % can be removed from appointment stream.Usually, this realizes in the following manner: lower area gaseous flow being fed to wash mill, the ullage of any liquid below the scrubbing tower of this lower area usually in this device but in the storage tank of wash mill, and one or more liquid stream (such as, organic solvent stream and current) are optionally fed to the upper zone of wash mill usually above scrubbing tower via rinse-system.The liquid column underflow comprising the derivative of organic solvent can be reclaimed from wash mill.Therefore, the one or more tower bottom flows comprising the derivative of organic solvent can be sent to oxidation reactor from cleaning section, with the recirculation of the derivative to oxidation reactor that realize organic solvent.Tower bottom flow can flow with other (such as, carrying out the liquid stream of the upper area of condenser or stripping tower) merges, and/or processed on its path to oxidation reactor.Alternatively, one or more tower bottom flow directly can be sent to oxidation reactor, that is, its path to oxidation reactor form to change it without undergoing any intermediate treatment.
Cleaning section can comprise the pressurized cleaner of the derivative of the organic solvent of the overhead gas that the emission gases for removing since oxidation reactor obtains, and at least one in the normal pressure washer of the derivative that removes the organic solvent from steam stream.Pressurized cleaner, usually under the pressure of at least 2.5barA or at least 5barA or at least 7.5barA or at least 10barA or at least 12.5barA, runs under being usually up to the pressure of 20barA or 30barA or 40barA or 50barA.Normal pressure washer, usually under the pressure of about 1barA, namely runs under about atmospheric pressure.Overhead gas obtains with the emission gases removing water and organic solvent always autoxidation section by making emission gases pass distilling period and condensation segment usually, and the material also comprised except the derivative of organic solvent as unreacting hydrocarbon precursor (such as, paraxylene).
As mentioned above, preferably first the organic solvent stream of purifying is cooled, then be fed to cleaning section, thus increase the recovery of derivative from gaseous flow of organic solvent further.This realizes by the heat (such as, in a heat exchanger) of the organic solvent stream from purifying being sent to the tower bottom flow transmitted by cleaning section (preferably from pressurized cleaner).This tower bottom flow can be sent to oxidation reactor subsequently afterwards.Control system can be comprised, the transport of this stream is back to air-lift device instead of oxidation reactor with another route when needed.Cold water charging can be used to be cooled further by the organic solvent stream of purifying and (such as, in a heat exchanger), to be fed to cleaning section subsequently.
The steam stream therefrom removing the derivative of organic solvent in normal pressure washer can be sent to normal pressure washer (that is, it can be the steam stream formed within the condenser) from condenser.Tower bottom flow from normal pressure washer can be sent to oxidation reactor.Can to the steam stream through washing from normal pressure washer, such as, in other scrubbing tower, water be used to be further processed.
Solvent air-lift device
The organic solvent of the pollution of the storage tank from air-lift device can be spread the solvent air-lift device delivered to and comprise distillation still and stripping tower, wherein will comprise the steam stream of the derivative of organic solvent, water and organic solvent and residue (such as, two or more mixture in M-phthalic acid, phthalic acid, p-methylbenzoic acid, benzoic acid, 4-carboxyl benzaldehyde, bromide (such as, hydrogen bromide), catalytic component or these components) be separated.Usually the organic solvent stream of pollution is sent to the stripping tower of solvent air-lift device as wash fluid.Steam from solvent air-lift device can be spread and deliver to air-lift device.
First process flow
First process flow can be selected from any one that guide in the above-mentioned stream of air-lift device, or can be another stream of the derivative comprising organic solvent, water and organic solvent.Particularly, first process flow can be selected from the first condensate flow obtained from the condensation of the vapor stream of top of the tower from the first crystallizer, the second condensate flow obtained from the condensation of the vapor stream of top of the tower from the second crystallizer, be fed to the organic solvent stream of the pollution of point higher air-lift device from the storage of the organic solvent polluted via external fluid passage, and from the steam stream of solvent air-lift device.
The disclosure is further described with reference to accompanying drawing.
Fig. 1 is the schematic diagram of the method and apparatus according to preferred embodiment of the present disclosure.Air-lift device 10 is made up of storage tank 20, stripping tower 30 and condenser 40, and they form integrated form unit.The lower area of storage tank 20 is divided into the storage 26 of the storage 24 of the organic solvent of purifying and the organic solvent of pollution by weir plate 22.Deflector 28 is arranged in above the storage 26 of the organic solvent of pollution, to make the storage 24 liquid fallen from stripping tower 30 being imported the organic solvent of purifying.Clean organic solvent (preferred acetic acid) flows 24b is fed to the organic solvent of purifying storage 24 via entrance.
The organic solvent stream 24a of purifying is removed to high-pressure pump 50 via outlet from the storage 24 of the organic solvent of purifying, the organic solvent stream 50a of purifying is sent to heat exchanger 70 by this high-pressure pump, and the organic solvent stream 50a of this purifying is cooled by pressurized cleaner tower bottom flow 80a in a heat exchanger.The organic solvent stream 70a of purifying is fed to pressurized cleaner 80, to be removed from the overhead gas stream 80b coming from oxidation reactor discharge gas stream 100a by organic solvent derivative (preferred methyl acetate).Pressurized cleaner discharge gas stream 80c is removed for further process.Pressurized cleaner tower bottom flow 70c is fed to oxidation reactor 100.The organic solvent stream 70b of purifying is fed to normal pressure washer 90, to be removed from condenser vapor stream 40b by the derivative of organic solvent.Normal pressure washer tower bottom flow 90a is fed to oxidation reactor 100.Normal pressure washer discharge currents 90b is removed for further process.
The organic solvent stream 26a of pollution is removed to low-lift pump 60 via the storage 26 of outlet from the organic solvent polluted.The organic solvent stream 60b of pollution is fed to solvent air-lift device 110.Steam stream 110a from solvent air-lift device 110 is fed to the entrance in storage tank 20 above deflector 28, and residual stream (not shown) is removed from solvent air-lift device 110.The organic solvent stream 60a of pollution is fed to the entrance in stripping tower 30.Liquid stream 40a is fed to oxidation reactor 100 from condenser 40.
Oxidation reactor product stream 100b is fed to the first crystallizer and the second crystallizer (not shown).The first condensate flow 20a condensation from the vapor stream of top of the tower from the first crystallizer and the second crystallizer obtained and the second condensate flow 20b is fed to the entrance in storage tank 20, and the liquid that described entrance is arranged to come from the first condensate flow 20a and the second condensate flow 20b enters the storage 26 of the organic solvent of pollution.
According to embodiment of the present disclosure, provide following equipment scheme.
Equipment scheme 1
For reclaiming an equipment for the derivative of organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
Equipment scheme 2
Equipment according to equipment scheme 1, wherein said stripping tower, storage tank and condenser form integrated form unit.
Equipment scheme 3
Equipment according to equipment scheme 1 or equipment scheme 2, wherein said storage tank also comprises the outlet of the organic solvent stream removing pollution.
Equipment scheme 4
Equipment according to equipment scheme 3, wherein said stripping tower also comprises the entrance of a part for the organic solvent stream receiving described pollution.
Equipment scheme 5
Equipment according to any one in equipment scheme 1-4, wherein said storage tank also comprises the first condensate flow entrance.
Equipment scheme 6
Equipment according to equipment scheme 5, wherein said first condensate flow entrance is between the storage of the organic solvent of described deflector and described pollution, and the liquid coming from the first condensate flow entering described first condensate flow entrance enters the storage of the organic solvent of described pollution.
Equipment scheme 7
Equipment according to equipment scheme 5, wherein said storage tank also comprises the second condensate flow entrance.
Equipment scheme 8
Equipment according to equipment scheme 7, wherein said second condensate flow entrance is between the storage of the organic solvent of described deflector and described pollution, and the liquid coming from the second condensate flow entering described second condensate flow entrance enters the storage of the organic solvent of described pollution.
Equipment scheme 9
Equipment according to any one in equipment scheme 1-6, wherein said storage tank also comprises the entrance for receiving clean organic solvent stream.
Equipment scheme 10
Equipment according to equipment scheme 9, the entrance wherein receiving described clean organic solvent stream makes described clean organic solvent flow to the storage of the organic solvent into described purifying.
Equipment scheme 11
Equipment according to any one in equipment scheme 1-10, wherein said first process flow entrance is in described stripping tower or in described storage tank.
Equipment scheme 12
Equipment according to any one in equipment scheme 1-11, the liquid flowing outlet that the liquid stream that the upper area of wherein said condenser or described stripping tower comprises the derivative by comprising described organic solvent removes from described air-lift device.
Equipment scheme 13
Equipment according to any one in equipment scheme 1-12, the vapor stream outlet that the steam stream of the derivative that wherein said condenser comprises comprising described organic solvent removes from described condenser.
Equipment scheme 14
Equipment according to any one in equipment scheme 1-13, wherein said stripping tower is destilling tower, described destilling tower comprises at least one theoretical separation stages, and at least one theoretical separation stages described is provided by other suitable structures on the surface of tower tray, structured packing or the quality transmission between the gas phase be provided in tower and liquid phase.
Equipment scheme 15
Equipment according to equipment scheme 14, wherein said tower tray is sieve tray, float valve tray or bubble cap tray.
Equipment scheme 16
For reclaiming an equipment for the derivative of organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Receive the air-lift device of the first process flow, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower, and
Prepare the oxidation reactor of aromatic dicarboxylic acid,
Wherein, described equipment also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
Equipment scheme 17
Equipment according to equipment scheme 16, described equipment also comprises
By the cleaning section that the derivative of described organic solvent removes from gaseous flow, and
The organic solvent stream of purifying is sent to described cleaning section with the device removed from described gaseous flow by the derivative of described organic solvent from described air-lift device.
Equipment scheme 18
Equipment according to equipment scheme 17, wherein said cleaning section comprises the derivative of described organic solvent from coming from the pressurized cleaner that removes from the overhead gas of the emission gases of described oxidation reactor and/or being drifted the normal pressure washer removed from steam by the derivative of described organic solvent.
Equipment scheme 19
Equipment according to equipment scheme 17 or equipment scheme 18, described equipment also comprises
One or more tower bottom flows are sent to the device of described oxidation reactor from described cleaning section.
Equipment scheme 20
Equipment according to any one in equipment scheme 17-19, described equipment also comprises the device of the organic solvent stream cooling described purifying.
Equipment scheme 21
Equipment according to equipment scheme 20, wherein said cleaning section comprises the pressurized cleaner from coming from the derivative removing described organic solvent from the overhead gas of the emission gases of described oxidation reactor, and the device of the organic solvent stream of the described purifying of described cooling comprises the device heat of the organic solvent stream from described purifying being sent to the tower bottom flow being sent to described oxidation reactor from described pressurized cleaner.
Equipment scheme 22
Equipment according to any one in equipment scheme 17-21, wherein said cleaning section comprises to drift the derivative of described organic solvent the normal pressure washer removed from the steam being sent to it by described condenser.
Equipment scheme 23
Equipment according to equipment scheme 21, described equipment also comprises
Solvent air-lift device,
The organic solvent stream of pollution is fed to the device of described solvent air-lift device from described storage tank, and
Steam stream is sent to the device of described air-lift device from described solvent air-lift device.
Equipment scheme 24
Equipment according to any one in equipment scheme 17-23, described equipment also comprises weir plate in the perpendicular that is separated with the storage of the organic solvent of pollution by the storage of the organic solvent of purifying.
Equipment scheme 25
Equipment according to equipment scheme 24, described equipment also comprises
First condensate flow of the condensation of the steam stream come from from the first crystallizer is fed to the device of described storage tank, the liquid coming from described first condensate flow enters the storage of the organic solvent of described pollution.
Equipment scheme 26
Equipment according to equipment scheme 25, described equipment also comprises
Second condensate flow of the condensation of the steam stream come from from the second crystallizer is fed to the device of described storage tank, the liquid coming from described second condensate flow enters the storage of the organic solvent of described pollution.
Equipment scheme 27
Equipment according to any one in equipment scheme 24-26, described equipment also comprises
The organic solvent stream of pollution is fed to the device of described stripping tower via external fluid path from the storage of the organic solvent of described pollution.
Equipment scheme 28
Equipment according to any one in equipment scheme 24-27, described equipment also comprises
Clean organic solvent stream is fed to the device of the storage of the organic solvent of described purifying.
Equipment scheme 29
For the preparation of an equipment for aromatic dicarboxylic acid, described equipment comprises
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow from the first crystallizer or the second crystallizer, the equipment of the described derivative from the first process flow recovery organic solvent from the first crystallizer or the second crystallizer comprises
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
Equipment scheme 30
For the preparation of an equipment for aromatic dicarboxylic acid, described equipment comprises
Prepare the oxidation reactor of aromatic dicarboxylic acid;
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow, the described equipment reclaiming the derivative of organic solvent from the first process flow comprises:
Receive the air-lift device of the first process flow, and described air-lift device comprises
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower,
The wherein said equipment reclaiming the derivative of organic solvent from the first process flow also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
In addition, in some embodiments, the disclosure also comprises following additional aspects.
Additional aspects 1
A kind of for the method from the derivative for the preparation of the first process flow recovery organic solvent in the method for aromatic dicarboxylic acid, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, the described method for the preparation of aromatic dicarboxylic acid comprises the catalytic oxidation of hydrocarbon precursor in described organic solvent in oxidation reactor, and the method for the derivative of described recovery organic solvent comprises the following steps:
I) described first process flow is fed to air-lift device, described air-lift device comprises stripping tower and storage tank air lift;
Ii) the organic solvent stream of purifying is removed from described storage tank; And
Iii) stripper overhead stream is sent to condenser from described stripping tower,
Wherein, step I i) in the purifying removed from described storage tank organic solvent stream the mass concentration of derivative of described organic solvent lower than step I) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device, and, optionally
Wherein, step I ii) in the mass concentration being sent to the derivative of the described organic solvent in the overhead streams of described condenser be greater than step I) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device.
Additional aspects 2
Method according to additional aspects 1, wherein said aromatic dicarboxylic acid is terephthalic acid (TPA).
Additional aspects 3
Method according to additional aspects 2, wherein said organic solvent is acetic acid.
Additional aspects 4
Method according to additional aspects 3, the derivative of wherein said organic solvent is methyl acetate.
Additional aspects 5
Method according to any one in front additional aspects, wherein said stripping tower, storage tank and condenser form integrated form unit.
Additional aspects 6
Method according to any one in front additional aspects, described method is further comprising the steps of:
Iv) liquid stream comprising the derivative of described organic solvent is fed to described oxidation reactor from the upper area of described condenser or described stripping tower.
Additional aspects 7
Method according to any one in front additional aspects, described method is further comprising the steps of:
V) the organic solvent stream of described purifying is fed to cleaning section, to be removed from gaseous flow by the derivative of described organic solvent.
Additional aspects 8
Method according to additional aspects 7, wherein said cleaning section comprises pressurized cleaner and/or normal pressure washer, described pressurized cleaner is used for the derivative of described organic solvent to remove from overhead gas, described overhead gas comes from the emission gases from described oxidation reactor, and described normal pressure washer is used for the derivative of described organic solvent to drift from steam to remove.
Additional aspects 9
Method according to additional aspects 7 or additional aspects 8, described method is further comprising the steps of:
Vi) one or more tower bottom flows are sent to described oxidation reactor from described cleaning section.
Additional aspects 10
Method according to any one in additional aspects 7-9, described method is further comprising the steps of:
Vii) cooled before the organic solvent stream of described purifying is fed to described cleaning section.
Additional aspects 11
Method according to additional aspects 10, wherein said cleaning section comprises pressurized cleaner, described pressurized cleaner is used for the derivative of described organic solvent to remove from overhead gas, described overhead gas comes from the emission gases from described oxidation reactor, and step vii) comprise and heat spread the tower bottom flow delivered to and be sent to described oxidation reactor from described pressurized cleaner from the organic solvent of described purifying.
Additional aspects 12
Method according to any one in additional aspects 7-11, wherein said cleaning section comprises normal pressure washer, and described normal pressure washer is used for the derivative of described organic solvent to drift from the steam being sent to described normal pressure washer by described condenser to remove.
Additional aspects 13
Method according to any one in front additional aspects, described method is further comprising the steps of:
Viii) the organic solvent stream of pollution is fed to solvent air-lift device from described storage tank; And
Ix) steam stream is sent to described air-lift device from described solvent air-lift device.
Additional aspects 14
Method according to any one in front additional aspects, wherein said storage tank comprises the interior weir plate of perpendicular, and the storage of the storage of the organic solvent of purifying with the organic solvent of pollution is separated by described interior weir plate.
Additional aspects 15
Method according to additional aspects 14, wherein said storage tank also comprises deflector, and described baffle arrangement is make the liquid from described stripping tower guide in the storage of the organic solvent of described purifying.
Additional aspects 16
Method according to additional aspects 14 or additional aspects 15, the mass concentration of the derivative of the described organic solvent in the organic solvent of wherein said pollution is more than or equal to about 2: 1 with the ratio of the mass concentration of the derivative of the described organic solvent in the organic solvent of described purifying, or be more than or equal to about 5: 1, or be more than or equal to about 7: 1.
Additional aspects 17
Method according to any one in additional aspects 14-16, described method is further comprising the steps of:
X) the first condensate flow of the condensation of the vapor stream of top of the tower come from from the first crystallizer is fed to the first condensate flow entrance in described storage tank, the liquid that described first condensate flow entrance is arranged to come from described first condensate flow enters the storage of the organic solvent of described pollution.
Additional aspects 18
Method according to additional aspects 17, described method is further comprising the steps of:
Xi) the second condensate flow of the condensation of the vapor stream of top of the tower come from from the second crystallizer is fed to the second condensate flow entrance in described storage tank, the liquid that described second condensate flow entrance is arranged to come from described second condensate flow enters the storage of the organic solvent of described pollution.
Additional aspects 19
Method according to any one in additional aspects 14-18, described method is further comprising the steps of:
Xii) organic solvent of the pollution of the storage of the organic solvent from described pollution is flowed through be fed to described stripping tower by external fluid path.
Additional aspects 20
Method according to any one in additional aspects 14-19, described method is further comprising the steps of:
Xiii) clean organic solvent stream is fed to the storage of the organic solvent of described purifying.
Additional aspects 21
For reclaiming an equipment for the derivative of organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device comprises:
Stripping tower;
Storage tank, described storage tank is arranged as and receives liquid from described stripping tower;
Condenser, described condenser is arranged as and receives overhead streams from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
The interior weir plate of perpendicular, the storage of the storage of the organic solvent of purifying with the organic solvent of pollution is separated by described interior weir plate;
Deflector, described baffle arrangement is the storage making the organic solvent liquid from described stripping tower being imported described purifying; And
The organic solvent flow export of purifying, described outlet is used for the organic solvent stream of purifying to remove from the storage of the organic solvent of described purifying.
Additional aspects 22
Equipment according to additional aspects 21, wherein said stripping tower, storage tank and condenser form integrated form unit.
Additional aspects 23
Equipment according to additional aspects 21 or additional aspects 22, wherein said storage tank also comprises the outlet of the organic solvent stream for removing pollution.
Additional aspects 24
Equipment according to additional aspects 23, wherein said stripping tower also comprises the entrance of a part for the organic solvent stream for receiving described pollution.
Additional aspects 25
Equipment according to any one in additional aspects 21-24, wherein said storage tank also comprises the first condensate flow entrance, wherein, optionally, described first condensate flow entrance is arranged between the storage of the organic solvent of described deflector and described pollution, and the liquid making to come from the first condensate flow entering described first condensate flow entrance enters the storage of the organic solvent of described pollution.
Additional aspects 26
Equipment according to additional aspects 25, wherein said storage tank also comprises the second condensate flow entrance, wherein, optionally, described second condensate flow entrance is arranged between the storage of the organic solvent of described deflector and described pollution, and the liquid making to come from the second condensate flow entering described second condensate flow entrance enters the storage of the organic solvent of described pollution.
Additional aspects 27
Equipment according to any one in additional aspects 21-26, wherein said storage tank also comprises the entrance for receiving clean organic solvent stream, wherein, optionally, the described entrance for receiving described clean organic solvent stream is arranged so that described clean organic solvent flows to the storage of the organic solvent into described purifying.
Additional aspects 28
Equipment according to any one in additional aspects 21-27, wherein said first process flow entrance is in described stripping tower or in described storage tank.
Additional aspects 29
Equipment according to any one in additional aspects 21-28, the upper area of wherein said condenser or described stripping tower comprises the liquid flowing outlet air lift that the liquid stream for the derivative by comprising described organic solvent removes from described air-lift device.
Additional aspects 30
Equipment according to any one in additional aspects 21-29, wherein said condenser comprises the vapor stream outlet that the steam stream for the derivative by comprising described organic solvent removes from described condenser.
Additional aspects 31
For reclaiming an equipment for the derivative of organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device is configured to reception first process flow, and described air-lift device comprises:
Stripping tower;
Storage tank, described storage tank is arranged as and receives liquid from described stripping tower; With
Condenser, described condenser is arranged as and receives overhead streams from described stripping tower, and oxidation reactor, and described oxidation reactor is used for the preparation of aromatic dicarboxylic acid, and the preparation of described aromatic dicarboxylic acid comprises the catalytic oxidation of hydrocarbon precursor in described organic solvent,
Wherein, described equipment also comprises:
Be sent to the device of described oxidation reactor from described condenser for the stream of the derivative by comprising described organic solvent.
Additional aspects 32
Equipment according to additional aspects 31, the wherein said stream comprising the derivative of described organic solvent is liquid stream.
Additional aspects 33
Equipment according to additional aspects 31 or additional aspects 32, described equipment also comprises:
For the cleaning section that the derivative of described organic solvent is removed from gaseous flow, and
For the organic solvent stream of purifying is sent to described cleaning section from described air-lift device, with the device removed from described gaseous flow by the derivative of described organic solvent.
Additional aspects 34
Equipment according to additional aspects 33, wherein said cleaning section comprises pressurized cleaner and/or normal pressure washer, described pressurized cleaner is used for the derivative of described organic solvent to remove from overhead gas, described overhead gas comes from the emission gases from described oxidation reactor, and described normal pressure washer is used for the derivative of described organic solvent to drift from steam to remove.
Additional aspects 35
Equipment according to additional aspects 33 or additional aspects 34, described equipment also comprises:
For one or more tower bottom flows to be sent to the device of described oxidation reactor from described cleaning section.
Additional aspects 36
Equipment according to any one in additional aspects 33-35, described equipment also comprises the device of the organic solvent stream for cooling described purifying.
Additional aspects 37
Equipment according to additional aspects 36, wherein said cleaning section comprises pressurized cleaner, described pressurized cleaner is used for the derivative removing described organic solvent from overhead gas, described overhead gas comes from the emission gases from described oxidation reactor, and comprises the device for the heat of the organic solvent stream from described purifying being sent to the tower bottom flow being sent to described oxidation reactor from described pressurized cleaner for the described device of the organic solvent stream cooling described purifying.
Additional aspects 38
Equipment according to any one in additional aspects 33-37, wherein said cleaning section comprises normal pressure washer, and described normal pressure washer is used for the derivative of described organic solvent to drift from the steam being sent to described normal pressure washer by described condenser to remove.
Additional aspects 39
Equipment according to additional aspects 38, described equipment also comprises:
Solvent air-lift device,
For the organic solvent stream of pollution to be fed to the device of described solvent air-lift device from described storage tank, and
For steam stream to be sent to the device of described air-lift device from described solvent air-lift device.
Additional aspects 40
Equipment according to any one in additional aspects 31-39, described equipment also comprises the interior weir plate of perpendicular, and the storage of the storage of the organic solvent of purifying with the organic solvent of pollution is separated by described interior weir plate.
Additional aspects 41
Equipment according to additional aspects 40, described equipment also comprises:
The first condensate flow for the condensation by the steam stream come from from the first crystallizer is fed to the device of described storage tank, and the liquid that described storage tank is arranged to come from described first condensate flow enters the storage of the organic solvent of described pollution.
Additional aspects 42
Equipment according to additional aspects 41, described equipment also comprises:
The second condensate flow for the condensation by the steam stream come from from the second crystallizer is fed to the device of described storage tank, and the liquid that described storage tank is arranged to come from described second condensate flow enters the storage of the organic solvent of described pollution.
Additional aspects 43
Equipment according to any one in additional aspects 40-42, described equipment also comprises:
For the organic solvent stream of pollution to be fed to the device of described stripping tower via external fluid path from the storage of the organic solvent of described pollution.
Additional aspects 44
Equipment according to any one in additional aspects 40-43, described equipment also comprises:
For clean organic solvent stream being fed to the device of the storage of the organic solvent of described purifying.Additional aspects 45
For a method for the preparation of aromatic dicarboxylic acid, described method comprises hydrocarbon precursor catalytic oxidation in organic solvent, said method comprising the steps of:
I) described hydrocarbon precursor is oxidized to provide aromatic dicarboxylic acid in described organic solvent under the existence of metallic catalyst;
Wherein said method is further comprising the steps of:
II) described the first process flow be used in the method for the preparation of aromatic dicarboxylic acid is fed to air-lift device, described air-lift device comprises stripping tower and storage tank, and described first process flow comprises the derivative of described organic solvent, water and described organic solvent;
III) the organic solvent stream of purifying is removed from described storage tank; And
IV) overhead streams is sent to condenser from described stripping tower,
Wherein, Step II I) in the purifying removed from described storage tank organic solvent stream the mass concentration of derivative of described organic solvent lower than Step II) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device, and, optionally
Wherein, step IV) in the mass concentration being sent to the derivative of the described organic solvent in the overhead streams of described condenser be greater than Step II) in the mass concentration being fed to the derivative of the described organic solvent in described first process flow of air-lift device.

Claims (30)

1., for reclaiming an equipment for the derivative of organic solvent from the first process flow, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
2. equipment according to claim 1, wherein said stripping tower, storage tank and condenser form integrated form unit.
3., according to equipment according to claim 1 or claim 2, wherein said storage tank also comprises the outlet of the organic solvent stream removing pollution.
4., according to equipment according to claim 1 or claim 2, wherein said stripping tower also comprises the entrance of a part for the organic solvent stream receiving described pollution.
5., according to equipment according to claim 1 or claim 2, wherein said storage tank also comprises the first condensate flow entrance.
6. equipment according to claim 5, wherein said first condensate flow entrance is between the storage of the organic solvent of described deflector and described pollution, and the liquid coming from the first condensate flow entering described first condensate flow entrance enters the storage of the organic solvent of described pollution.
7. equipment according to claim 5, wherein said storage tank also comprises the second condensate flow entrance.
8. equipment according to claim 7, wherein said second condensate flow entrance is between the storage of the organic solvent of described deflector and described pollution, and the liquid coming from the second condensate flow entering described second condensate flow entrance enters the storage of the organic solvent of described pollution.
9., according to equipment according to claim 1 or claim 2, wherein said storage tank also comprises the entrance for receiving clean organic solvent stream.
10. equipment according to claim 9, the entrance wherein receiving described clean organic solvent stream makes described clean organic solvent flow to the storage of the organic solvent into described purifying.
11. according to equipment according to claim 1 or claim 2, and wherein said first process flow entrance is in described stripping tower or in described storage tank.
12. according to equipment according to claim 1 or claim 2, the liquid flowing outlet that the liquid stream that the upper area of wherein said condenser or described stripping tower comprises the derivative by comprising described organic solvent removes from described air-lift device.
13. according to equipment according to claim 1 or claim 2, the vapor stream outlet that the steam stream of the derivative that wherein said condenser comprises comprising described organic solvent removes from described condenser.
14. according to equipment according to claim 1 or claim 2, wherein said stripping tower is destilling tower, described destilling tower comprises at least one theoretical separation stages, and at least one theoretical separation stages described is provided by other suitable structures on the surface of tower tray, structured packing or the quality transmission between the gas phase be provided in tower and liquid phase.
15. equipment according to claim 14, wherein said tower tray is sieve tray, float valve tray or bubble cap tray.
16. 1 kinds of equipment for the derivative from the first process flow recovery organic solvent, described first process flow comprises the derivative of described organic solvent, water and described organic solvent, and described equipment comprises:
Receive the air-lift device of the first process flow, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower, and
Prepare the oxidation reactor of aromatic dicarboxylic acid,
Wherein, described equipment also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
17. equipment according to claim 16, described equipment also comprises
By the cleaning section that the derivative of described organic solvent removes from gaseous flow, and
The organic solvent stream of purifying is sent to described cleaning section with the device removed from described gaseous flow by the derivative of described organic solvent from described air-lift device.
18. equipment according to claim 17, wherein said cleaning section comprises the derivative of described organic solvent from coming from the pressurized cleaner that removes from the overhead gas of the emission gases of described oxidation reactor and/or being drifted the normal pressure washer removed from steam by the derivative of described organic solvent.
19. according to claim 17 or equipment according to claim 18, and described equipment also comprises
One or more tower bottom flows are sent to the device of described oxidation reactor from described cleaning section.
20. according to claim 17 or equipment according to claim 18, and described equipment also comprises the device of the organic solvent stream cooling described purifying.
21. equipment according to claim 20, wherein said cleaning section comprises the pressurized cleaner from coming from the derivative removing described organic solvent from the overhead gas of the emission gases of described oxidation reactor, and the device of the organic solvent stream of the described purifying of described cooling comprises the device heat of the organic solvent stream from described purifying being sent to the tower bottom flow being sent to described oxidation reactor from described pressurized cleaner.
22. according to claim 17 or equipment according to claim 18, and wherein said cleaning section comprises to drift the derivative of described organic solvent the normal pressure washer removed from the steam being sent to it by described condenser.
23. equipment according to claim 21, described equipment also comprises
Solvent air-lift device,
The organic solvent stream of pollution is fed to the device of described solvent air-lift device from described storage tank, and
Steam stream is sent to the device of described air-lift device from described solvent air-lift device.
24. according to claim 17 or equipment according to claim 18, and described equipment also comprises weir plate in the perpendicular that is separated with the storage of the organic solvent of pollution by the storage of the organic solvent of purifying.
25. equipment according to claim 24, described equipment also comprises
First condensate flow of the condensation of the steam stream come from from the first crystallizer is fed to the device of described storage tank, the liquid coming from described first condensate flow enters the storage of the organic solvent of described pollution.
26. equipment according to claim 25, described equipment also comprises
Second condensate flow of the condensation of the steam stream come from from the second crystallizer is fed to the device of described storage tank, the liquid coming from described second condensate flow enters the storage of the organic solvent of described pollution.
27. equipment according to claim 24, described equipment also comprises
The organic solvent stream of pollution is fed to the device of described stripping tower via external fluid path from the storage of the organic solvent of described pollution.
28. equipment according to claim 24, described equipment also comprises
Clean organic solvent stream is fed to the device of the storage of the organic solvent of described purifying.
29. 1 kinds of equipment for the preparation of aromatic dicarboxylic acid, described equipment comprises
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow from the first crystallizer or the second crystallizer, the equipment of the described derivative from the first process flow recovery organic solvent from the first crystallizer or the second crystallizer comprises
Air-lift device, described air-lift device comprises:
Stripping tower;
The storage tank of liquid is received from described stripping tower;
The condenser of overhead streams is received from described stripping tower; And
First process flow entrance;
Wherein said storage tank comprises
Weir plate in the perpendicular that the storage of the organic solvent of purifying is separated with the storage of the organic solvent of pollution;
Liquid from described stripping tower is imported the deflector of the storage of the organic solvent of described purifying; And
By the organic solvent flow export of the purifying that the organic solvent stream of purifying removes from the storage of the organic solvent of described purifying.
30. 1 kinds of equipment for the preparation of aromatic dicarboxylic acid, described equipment comprises
Prepare the oxidation reactor of aromatic dicarboxylic acid;
First crystallizer;
Second crystallizer;
Reclaim the equipment of the derivative of organic solvent from the first process flow, the described equipment reclaiming the derivative of organic solvent from the first process flow comprises:
Receive the air-lift device of the first process flow, and described air-lift device comprises
Stripping tower;
The storage tank of liquid is received from described stripping tower; With
The condenser of overhead streams is received from described stripping tower,
The wherein said equipment reclaiming the derivative of organic solvent from the first process flow also comprises:
The stream comprising the derivative of described organic solvent is sent to the device of described oxidation reactor from described condenser.
CN201520107979.2U 2014-10-07 2015-02-13 For reclaiming the equipment of derivative of organic solvent and the equipment for the preparation of aromatic dicarboxylic acid from the first process flow Active CN204637629U (en)

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WO1998045239A1 (en) * 1997-04-09 1998-10-15 E.I. Du Pont De Nemours And Company Water separation process
US6150553A (en) * 1998-08-11 2000-11-21 E. I. Du Pont De Nemours And Company Method for recovering methyl acetate and residual acetic acid in the production acid of pure terephthalic acid
TW483886B (en) * 1998-08-11 2002-04-21 Du Pont Method for recovering methyl acetate and residual acetic acid in the production of pure terephtalic acid
AU2004213274A1 (en) * 2003-02-21 2004-09-02 Astellas Pharma Inc Process for producing aromatic carboxylic acid
CN1867537B (en) * 2003-08-12 2013-06-05 Amt国际股份有限公司 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
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GB201417735D0 (en) 2014-11-19

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