CN105985237A - Production of an aromatic dicarboxylic acid - Google Patents
Production of an aromatic dicarboxylic acid Download PDFInfo
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- CN105985237A CN105985237A CN201510079766.8A CN201510079766A CN105985237A CN 105985237 A CN105985237 A CN 105985237A CN 201510079766 A CN201510079766 A CN 201510079766A CN 105985237 A CN105985237 A CN 105985237A
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- serosity
- heat
- dicarboxylic acid
- aromatic dicarboxylic
- steam
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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
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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
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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
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a method for raising steam in a process for the production of an aromatic dicarboxylic acid comprising the catalytic oxidation of a hydrocarbon precursor in an organic solvent, comprising the steps of: i) heating a crude aromatic dicarboxylic acid slurry to form a crude aromatic dicarboxylic acid solution; ii) transferring the crude aromatic dicarboxylic acid solution to a hydrogenation reactor; iii) transferring a purified aromatic dicarboxylic acid solution from the hydrogenation reactor to a series of one or more crystallisers; and iv) transferring heat from a crystalliser vent stream from the series of one or more crystallisers to a water stream in a steam raiser to generate steam. 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 preparation in organic solvent of hydrocarbon precursor.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 making 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 of PTA manufacture 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.
Generally it is introduced to heat in aromatic dicarboxylic acid maker and uses steam to make carrier wherein pass
Send heat.Specifically, by combustion heating fuel to add hot water (such as in fossil-fuel boiler),
The high-pressure steam that temperature is e.g., from about 300 DEG C can be generated outside battery limits, then this water under high pressure is steamed
Conductance is to one or more heat exchangers, to transfer heat to the technique stream with maximum temperature demand.
The high pressure condensate of gained can be carried out flash distillation with mesohigh that preparation temperature is e.g., from about 220 DEG C
Steam (intermediate-pressure steam), then this mesohigh steam can be used for heating and has
The technique stream of relatively low heat demand forms mesohigh condensate (intermediate-pressure condensate),
This mesohigh condensate can be carried out flash distillation with setting-out steam in preparation, the most and so forth until institute
Till stating the depleted of energy of steam.
Significantly may be used of heating fuel mix aromatic dicarboxylic acid manufacture method needed for generating high-pressure steam
Become this.It is an object of the invention to provide a kind of for manufacturing more economically and more having of aromatic dicarboxylic acid
Effect method and apparatus and, specifically, the high-pressure steam of aromatic dicarboxylic acid manufacture method will be used for
Demand minimizes.Further purpose will be clear to from description below.
Summary of the invention
This purpose can (such as mesohigh water steams by generating the steam of relatively low pressure in the process
Gas) realize rather than by directly obtaining these steam from high-pressure steam.Therefore the present invention
First aspect provide a kind of side for generating steam in the method prepare aromatic dicarboxylic acid
Method, the described method preparing aromatic dicarboxylic acid includes the catalysis oxidation in organic solvent of hydrocarbon precursor, institute
The method stating generation steam comprises the following steps:
I) thick aromatic dicarboxylic acid serosity is heated to form thick aromatic dicarboxylic acid solution；
Ii) described thick aromatic dicarboxylic acid solution is sent to hydrogenation reactor；
Iii) the aromatic dicarboxylic acid solution of purification is sent to a series of one from described hydrogenation reactor
Or multiple crystallizer；And
Iv) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current in steam maker are to generate steam.
The steam generated is usually saturated steam.Preferably, in step iv) the middle water generated
Steam is middle setting-out steam or mesohigh steam.It is highly preferred that in step iv) the middle water steaming generated
Gas is mesohigh steam.
As used herein, " high-pressure steam " is that finger pressure is about 50-150barA or about 75-125
The saturated steam of barA or about 100barA.Similarly, " high pressure condensate " is that finger pressure is
The condensate of about 50-150barA or about 75-125barA or about 100barA.As made herein
With, " mesohigh steam " is that finger pressure is about 10-50barA or about 12.5-40barA or about
The saturated steam of 15-35barA or about 17.5-30barA or about 20barA.As made herein
With, " middle setting-out steam " is that finger pressure is about 5-10barA or about 6-9barA or about 8barA
Saturated steam.As used herein, " Low pressure steam " is that finger pressure is less than about 5barA
Saturated steam.
Thick aromatic dicarboxylic acid serosity can use high-pressure steam to heat.Therefore, step i) can include step
V): the thick aromatic dicarboxylic acid slurry that heat is sent to the first serosity heat exchanger from high-pressure steam
Liquid.High pressure condensate can generate in step v).High pressure condensate is generally in and steams with water under high pressure
At a temperature of gas is substantially the same, such as high pressure condensate can be at lower 10 DEG C than high-pressure steam,
Or at a temperature of low 5 DEG C.Such as, if high-pressure steam is at a temperature of 290-320 DEG C, then
High pressure condensate can be at a temperature of 280-310 DEG C, or 285-315 DEG C.Therefore, step i) is also
Step vi can be included): in the second serosity heat exchanger, heat is sent to institute from described high pressure condensate
Stating thick aromatic dicarboxylic acid serosity, described second serosity heat exchanger is starched relative to described thick aromatic dicarboxylic acid
The flow direction of liquid is arranged in the upstream of described first serosity heat exchanger.Relative to described thick aromatics dicarboxyl
The upstream of the described second serosity heat exchanger of the flow direction of Calyx seu fructus physalis liquid, can be by thick aromatic dicarboxylic acid serosity
It is heated at least 250 DEG C, it is preferable that directly that heat is the coldest from described high-pressure steam or described high pressure
Condensate is sent to described thick aromatic dicarboxylic acid serosity.Therefore, will be from described high pressure condensate and institute
The heat stating high-pressure steam applied before described thick aromatic dicarboxylic acid serosity, so that it may by described thick aromatics
Dicarboxylic acids serosity is heated to high temperature.Then, before described stream arrives at described hydrogenation reactor, described
The last increase in temperature needed for high pressure condensate and the offer of described high-pressure steam.Therefore, therewith
Before manufacture method and maker compare, the present invention by more economically, effective and favourable in the way of use
High-pressure steam.
This aspect of the invention additionally provides a kind of for generating in the method prepare aromatic dicarboxylic acid
The equipment of steam, the described method preparing aromatic dicarboxylic acid includes hydrocarbon precursor urging in organic solvent
Changing oxidation, described equipment includes:
A) the first serosity heat exchanger, described first serosity heat exchanger arrangement is for receiving thick aromatics dicarboxyl
Calyx seu fructus physalis liquid；
B) hydrogenation reactor, described hydrogenation reactor is configured to receive from described first serosity heat exchange
The thick aromatic dicarboxylic acid solution of device；
C) a series of one or more crystallizer, the one or more crystallizer is configured to receive
Aromatic dicarboxylic acid solution from the purification of described hydrogenation reactor；And
D) steam maker, described steam maker is configured to heat from from the one of described series
Individual or multiple crystallizer crystallizer discharge stream is sent to current to generate steam.
The steam generated is usually saturated steam.Preferably, raw by steam maker d)
The steam become is middle setting-out steam or mesohigh steam.It is highly preferred that by steam maker
D) steam generated is mesohigh steam.
High-pressure steam can be used to heat thick aromatic dicarboxylic acid serosity.Therefore, the first serosity heat exchange
Device is configurable to from high-pressure steam, heat is sent to thick aromatic dicarboxylic acid serosity.Described equipment also may be used
Including e) the second serosity heat exchanger, described second serosity heat exchanger arrangement is from by high pressure by heat
The high pressure condensate that steam generates is sent to thick aromatic dicarboxylic acid serosity, and relative to thick aromatics two
The flow direction of carboxylic acid slurry is arranged in the upstream of the first serosity heat exchanger.Described equipment is configurable to
Relative to the upstream of described second serosity heat exchanger of the flow direction of thick aromatic dicarboxylic acid serosity by described
Thick aromatic dicarboxylic acid serosity is heated at least 250 DEG C, it is preferable that the most directly by heat from high-pressure steam
Or high pressure condensate is sent to thick aromatic dicarboxylic acid serosity.Therefore, will be from high pressure condensate and height
The heat of setting-out steam applied before thick aromatic dicarboxylic acid serosity, can be added by thick aromatic dicarboxylic acid serosity
Heat is to high temperature.Then, before described stream arrives at hydrogenation reactor, high pressure condensate and high-pressure steam
Temperature required last increase is provided.
The present inventor is it has surprisingly found that can use and be thermally generated water from crystallizer discharge stream
Steam (specifically mesohigh steam), and do not increase in the method high-pressure steam elsewhere
Demand, such as, need not other high-pressure steam and (be not used for compared to wherein crystallizer discharge stream raw
The method becoming steam) heat thick aromatic dicarboxylic acid serosity.Therefore, the invention provides new water
Vapor source, specifically mesohigh steam, it can be used for substituting the steam deriving from high-pressure steam,
Therefore compared to previous manufacture method and equipment, the present invention is with one more economically, effectively and favorably
Mode use high-pressure steam, and decrease the overall high-pressure steam demand of described method, this
Then decrease demand for heat and therefore reduce variable cost.
Therefore, a second aspect of the present invention provides a kind of for adding in the method prepare aromatic dicarboxylic acid
The method of hot gas stream, the described method preparing aromatic dicarboxylic acid includes that hydrocarbon precursor is in organic solvent
Catalysis oxidation, described in add the method for hot gas stream and comprise the following steps:
I) steam is generated by method according to the first aspect of the invention；And
II) heat is sent to the gas stream described first gas heat-exchanger from described steam.
This aspect of the invention additionally provides a kind of for heating in the method prepare aromatic dicarboxylic acid
The equipment of gas stream, the described method preparing aromatic dicarboxylic acid includes hydrocarbon precursor urging in organic solvent
Changing oxidation, described equipment includes:
A) for generating the equipment of steam according to the first aspect of the invention；And
B) the first gas heat-exchanger, described first gas heat-exchanger is configured to steam heat from described water
Gas is sent to described gas stream.
Gas stream can be pressurization scrubber discharge gas stream.It is necessary that first heating this gas stream is passed again
Deliver in catalytic burner, wherein organic compound is removed from this gas stream.Therefore, the present invention carries
High-pressure steam demand elsewhere is not the most increased in described method for not high-pressure steam
The method heating this stream, thus decrease the overall high-pressure steam demand of described method.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the method and apparatus according to 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 to go the 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
In the method and apparatus of the present invention, the aromatic dicarboxylic acid of preparation is preferably selected from p-phthalic acid, adjacent benzene
Dioctyl phthalate and M-phthalic acid.Aromatic dicarboxylic acid is preferably p-phthalic acid.Hydrocarbon precursor is oxidable shape
Become the compound of aromatic dicarboxylic acid.Therefore, hydrocarbon precursor is usually the carboxylic acid in required end product
The position of substituent group is by such as C1-6The substituted benzene of alkyl, formoxyl or acetyl group or naphthalene.Preferably before hydrocarbon
Body is C1-6The substituted benzene of alkyl, specifically, for xylol.Organic solvent is usually aliphatic carboxylic acid,
Such as acetic acid, or the mixture of one or more these type of aliphatic carboxylic acids and water.Oxidation reaction can have wherein
Oxygen any under the conditions of carry out, such as, this reaction can be carried out in atmosphere.Catalysts is usual
Comprise cobalt and/or the manganese (such as, their acetate) of soluble form, use bromine source (such as hydrogen bromide)
As accelerator.The temperature of oxidation reaction is generally in the range of about 100-250 DEG C, it is therefore preferable to about
150-220℃.The pressure of any routine can be used in this reaction, with suitably by this reactant mixture
Keep 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.Product stream is generally sent to crystallized region to form the first slurry of thick aromatic dicarboxylic acid crystal
Liquid and overhead vapours.Generally the first serosity of thick aromatic dicarboxylic acid crystal is sent to segregation section, wherein
Mother solution is separated with thick aromatic dicarboxylic acid crystal, then can mix to form thick virtue with liquid, aqueous
Second serosity of race's dicarboxylic acid crystals.Generally the second serosity of this thick aromatic dicarboxylic acid crystal is sent to
Purification devices, heats and hydrogenates, and cools 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.
Thick aromatic dicarboxylic acid serosity
As it has been described above, the serosity of the thick aromatic dicarboxylic acid crystal in liquid, aqueous is carried out typical aromatics
The purification section of dicarboxylic acids manufacture method.Therefore, in this type of method, above-mentioned thick aromatic dicarboxylic acid crystal
The second serosity form the thick aromatic dicarboxylic acid serosity used in the present invention.This serosity is except comprising virtue
Outside race's dicarboxylic acids, the most also comprise byproduct of reaction (such as TA preparation in p-methylbenzoic acid,
Benzoic acid and 4-CBA) and organic solvent derivant and (such as from the methyl acetate of acetic acid)
With a small amount of catalysts.Heat thick aromatic dicarboxylic acid serosity to form thick aromatic dicarboxylic acid solution,
This solution carries out in hydrogenation reactor hydrogenation, and generally on carbon, the fixed bed of the palladium of load is urged
By some in agent, under high temperature (such as 275-290 DEG C) and high pressure (such as 70-90barA)
Impurity changes into the form being easier to remove from the aromatic dicarboxylic acid crystal of purification and (such as will
4-CBA is converted into p-methylbenzoic acid).
Heating serosity
Generally before the hydrogenation of the thick aromatic dicarboxylic acid solution of gained, first by thick aromatic dicarboxylic acid serosity
Heating is to dissolve byproduct of reaction, generally up to about 280 DEG C or higher temperature.This can pass through
Heat is streamed to a series of heat exchanger (such as shell-tube type heat exchange from what series of temperature gradually rose
Device) in serosity realize.Therefore, along with by thick aromatic dicarboxylic acid serosity by this series of temperatures gradually
The stream heating raised, the solid in thick aromatic dicarboxylic acid serosity dissolves so that ultimately form thick aromatics two
Carboxylic acid solution.First heat exchanger (counting up from hydrogenation reactor) applies finally to add before the hydrogenation
Hot step, and this be generally used in outside battery limits generate high-pressure steam source carry out, this water under high pressure
The temperature of vapor source is e.g., from about 300 DEG C.Therefore, heat is sent to the first serosity from high-pressure steam
Thick aromatic dicarboxylic acid serosity in heat exchanger.Because the generation of this high-pressure steam constitutes aromatics two
The significant variable cost of carboxylic acid manufacture method, it is desirable to farthest reduce the high pressure of the method
Steam demand also farthest utilizes the heat energy from this steam.Therefore, can be by this
The high pressure condensate generated in first hot transfer step is sent to the second heat exchanger (relative to thick aromatics
The flow direction of dicarboxylic acids serosity is arranged in the upstream of the first serosity heat exchanger), in the second heat exchanger
Heat is sent to thick aromatic dicarboxylic acid serosity from high pressure condensate.
Before thick aromatic dicarboxylic acid serosity arrives at the second heat exchanger, by by described thick aromatics dicarboxyl
The preheating of Calyx seu fructus physalis liquid can partly reduce the high-pressure steam demand of described heating steps.Therefore, in phase
For the upstream of the second serosity heat exchanger of the flow direction of described thick aromatic dicarboxylic acid serosity, can be by thick
Aromatic dicarboxylic acid serosity is heated at least 220 DEG C or at least 230 DEG C or at least 240 DEG C, or excellent
Selection of land at least 250 DEG C, it is preferable that the most directly heat is sent to from high-pressure steam or high pressure condensate
Thick aromatic dicarboxylic acid serosity.Can by by heat from one of the one or more crystallizers from this series
Individual or multiple crystallizer discharge stream are sent to the thick aromatics two in one or more other heat exchanger
Carboxylic acid slurry carries out this preheating.Therefore, the step heating thick aromatic dicarboxylic acid serosity can also include
Heat is sent to the 3rd serosity from the crystallizer discharge stream of the one or more crystallizers from this series
Thick aromatic dicarboxylic acid serosity in heat exchanger, described 3rd serosity heat exchanger is relative to thick aromatics two
The flow direction of carboxylic acid slurry is arranged in the upstream of the second serosity heat exchanger.
The present invention can include being sent to a series of from hydrogenation reactor by the aromatic dicarboxylic acid solution of purification
Two or more crystallizer a series of three devices crystallized above or a series of more than four knot
Brilliant device or a series of five devices crystallized above.
" first " crystallizer in a series of is the aromatics dicarboxyl receiving the purification from hydrogenation reactor
The crystallizer of acid solution.Therefore, it can heat from from the crystallizer row of the first crystallizer this series
Release the thick aromatic dicarboxylic acid serosity being sent in the 3rd serosity heat exchanger.Alternately, or additionally,
Heat can be sent to the 3rd serosity from the crystallizer discharge stream from the second crystallizer this series
Thick aromatic dicarboxylic acid serosity in heat exchanger.The step heating thick aromatic dicarboxylic acid serosity can also be wrapped
Include and heat is sent to the 4th slurry from the crystallizer discharge stream of the one or more crystallizers from this series
Thick aromatic dicarboxylic acid serosity in liquid heat exchanger, described 4th serosity heat exchanger is relative to thick aromatics
The flow direction of dicarboxylic acids serosity is arranged in the upstream of the 3rd serosity heat exchanger.Specifically, can by heat from
In this series, the crystallizer discharge stream of the second crystallizer is sent in the 4th serosity heat exchanger
Thick aromatic dicarboxylic acid serosity.
Single discharge stream can be obtained from each of above-mentioned crystallizer and be sent to above-mentioned heat friendship
Parallel operation.Alternatively, multiple discharge stream can be obtained from each of above-mentioned crystallizer (by making apparatus
There is the crystallizer of multiple steam vent, or by segmentation from the single steam vent in each crystallizer
Stream), then in multiple discharge stream is sent to above-mentioned heat exchanger, and by other or
Multiple (such as, be used for generate steam) elsewhere being used in described method.
Steam maker
Steam maker is heat exchanger, preferably shell-and-tube exchanger (such as autoclave heat exchanger),
Wherein from crystallizer discharge stream, heat is sent to current (such as, boiler feed water stream) steam to generate water
Gas, preferably mesohigh steam.Generally current are pumped under stress steam maker, and
Can also be preheated before current are sent to steam maker.
Although the heat of the crystallizer discharge stream from the first crystallizer in this series can be sent to
Current in steam maker, but this crystallizer discharge stream generally ratio is used for generating mesohigh water
Steam required hotter, heating thick aromatic dicarboxylic acid serosity hence with this crystallizer discharge stream is
More effectively.It is therefore preferable that by heat from the second crystallizer this series or this series
The current that are sent in steam maker of the crystallizer discharge stream of later crystallization device steam to generate water
Gas.Specifically, it is preferred that heat is spread from from the crystallizer discharge of the second crystallizer this series
Deliver to the current in steam maker to generate steam.Although than the first crystallization in this series
The crystallizer discharge stream of device is colder, but is in from the crystallizer discharge stream of the second crystallizer and be enough to generate
Under the high temperature of mesohigh steam.If it may further be preferable that by heat from from this series
The thick aromatic dicarboxylic acid slurry that the crystallizer discharge stream of two crystallizers is sent in the 4th serosity heat exchanger
Liquid, and heat is sent to steam from the crystallizer discharge stream from the second crystallizer this series
Current in maker are to generate steam.This can be used for guaranteeing that the generation of steam does not include thick aromatics
The generation of the heating of dicarboxylic acids serosity, i.e. steam does not results in needs other high-pressure steam heating
Thick aromatic dicarboxylic acid serosity.
Add hot gas stream
The steam (such as mesohigh steam) generated in a first aspect of the present invention can be used for adding
Heat other streams in the method and apparatus preparing aromatic dicarboxylic acid, thus reduce other steam,
The use of the most valuable high-pressure steam.Therefore, a second aspect of the present invention by by heat from
The gas stream that described steam is sent in the first gas heat-exchanger uses this steam.
Described steam, specifically mesohigh steam, have been observed that heating pressurization scrubber's discharge
Gas stream is particularly useful.Pressurization scrubber is in a series of segments, and these sections are for will be from
It was processed before atmospheric environment by the overhead gas release of condensation segment.This equipment is first with organic
Solvent (such as acetic acid) then washes overhead gas with water, thus reduces the material in described gas such as
Unreacted hydrocarbon precursor (such as xylol) and organic solvent derivant (such as methyl acetate)
Level.Then discharge gas stream in pressurization scrubber can be further processed.For example, it is possible to urging
Change and burner processes this gas stream to remove carbon monoxide and the organic component of any remnants, then
The catalytic burner exit gas of gained can be processed in exhaust scrubber further, then release into
In atmospheric environment.
Wish before it is further processed, first heating pressurization scrubber's discharge gas stream, as
Catalysis burning, to increase these efficiency processed.Can be by pressurization scrubber discharge gas stream second
Gas heat-exchanger preheats (such as by by the heat transmission from Low pressure steam or middle setting-out steam
To the second gas heat-exchanger), described second gas heat-exchanger is relative to pressurization scrubber discharge gas
The flow direction of body stream is arranged in the upstream of the first gas heat-exchanger.Alternately, or additionally, can be
In three gas heat-exchangers by heat is sent to pressurize scrubber discharge gas stream it is added
Heat, described 3rd gas heat-exchanger is arranged in the relative to the flow direction of pressurization scrubber discharge gas stream
The downstream of one gas heat-exchanger.Therefore, it can pressurization scrubber discharge gas stream from the first gas
Heat exchanger is sent to the 3rd gas heat-exchanger, then can be sent to urge from the 3rd gas heat-exchanger
Change burner.The catalytic burner exit gas of in the future self-catalysis burner can be streamed to the 3rd gas
Heat exchanger, so that being streamed to, from catalytic burner exit gas, scrubber's discharge gas that pressurizes by heat
Body stream.
The present invention will be further described with reference to the drawings.
Fig. 1 is the schematic diagram of the method and apparatus according to the preferred embodiments of the invention.Bringing-up section
10 include the first heat exchanger the 12, second heat exchanger the 14, the 3rd heat exchanger 16 and the 4th heat
Exchanger 18.First heat exchanger 12 is supplied with pressure and is about the high-pressure steam charging of 100barA
12a, this charging generates in the boiler of fossil fuel fired, (the most right to heat thick aromatic dicarboxylic acid
Phthalic acid) slurry stream 14a.High pressure condensate flow 12b is sent to the second heat exchanger 14 with
Heat thick aromatic dicarboxylic acid slurry stream 16a.By crystallizer discharge stream 30a from the first crystallizer 30
Feed to the 3rd heat exchanger 16 to heat thick aromatic dicarboxylic acid slurry stream 18a.Will be from the second knot
Crystallizer discharge stream 40a of brilliant device 40 feeds to the 4th heat exchanger 18 to heat thick aromatic dicarboxylic acid
Slurry stream 10a.Therefore, thick aromatic dicarboxylic acid slurry stream 10a is fed to bringing-up section 10, and will
This serosity is successively the 4th heat exchanger 18, the 3rd heat exchanger the 16, second heat exchanger 14 and
One heat exchanger 12 heats to dissolve its solid constituent thus forms thick aromatic dicarboxylic acid solution stream
10b.Heating should make thick aromatic dicarboxylic acid slurry stream 16a temperature when arriving the second heat exchanger 14 be
At least 250 DEG C.
By thick aromatic dicarboxylic acid solution stream 10b feed to hydrogenation reactor 20, in this reactor
On carbon on the fixed bde catalyst of the palladium of load, in the pressure of the temperature of 275-290 DEG C and 70-90barA
Under power, thick aromatic dicarboxylic acid solution stream 10b is carried out hydrogenation.By the aromatic dicarboxylic acid solution of purification
Stream 20a feeds to the first crystallizer 30 to form aromatic dicarboxylic acid slurry stream 30b of purification, should
Slurry stream feeds to the second crystallizer 40.Remove purification aromatic dicarboxylic acid slurry stream 40b for
Process further, to reclaim the aromatic dicarboxylic acid crystal of purification.
Crystallizer from the second crystallizer 40 is discharged steam 40c feed to steam maker
50 with heating boiler feed water stream 50a.Pressure is about the mesohigh steam charging 50b of 22barA
Feed to the first gas heat-exchanger 60 with heating pressurization scrubber's discharge gas stream 70d.By low
Setting-out vapor feed 70b heats discharge gas stream in pressurization scrubber in the second gas heat-exchanger 70
70a, and pressurization scrubber discharge gas stream 70d is sent to the first gas heat-exchanger 60.Will
Discharge gas stream 60a in pressurization scrubber feeds to the 3rd gas heat-exchanger 80.To pressurize scrubber
Discharge gas stream 80a feeds to catalytic burner 90 to prepare catalytic burner exit gas stream 90a,
This gas is flow to material and is back to the 3rd gas heat-exchanger 80, with heating pressurization scrubber's discharge gas
Body stream 60a.By catalytic burner exit gas stream 80b by being used for Power Recovery (power recovery)
Exhaust gas expander, be the most first emitted into exhaust scrubber and be released into again in atmospheric environment.
Collect waste water steam 16b, 18b and 50c and be recycled back processing equipment.By waste water steam/
Condensate 14b, 60b and 70c feed to steam recovery system for future use.
Embodiment according to the disclosure, it is provided that below scheme.
Scheme 1
A kind of method for generating steam in the method prepare aromatic dicarboxylic acid, described preparation virtue
The method of race's dicarboxylic acids includes the catalysis oxidation in organic solvent of hydrocarbon precursor, described generation steam
Method comprises the following steps:
I) thick aromatic dicarboxylic acid serosity is heated to form thick aromatic dicarboxylic acid solution；
Ii) described thick aromatic dicarboxylic acid solution is sent to hydrogenation reactor；
Iii) the aromatic dicarboxylic acid solution of purification is sent to a series of one from described hydrogenation reactor
Or multiple crystallizer；And
Iv) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current in steam maker are to generate steam.
Scheme 2
According to the method described in scheme 1, wherein in step iv) in generate steam be middle setting-out steam
Gas or mesohigh steam.
Scheme 3
According to the method described in scheme 2, wherein in step iv) in generate steam be mesohigh water
Steam.
Scheme 4
According to the method described in scheme 2 or scheme 3, the pressure of wherein said mesohigh steam is about
10-50BarA or about 12.5-40barA or about 15-35BarA or about 17.5-30barA or
About 20BarA.
Scheme 5
According to the method described in any one in scheme 1-4, wherein step i) comprises the following steps:
V) the described thick aromatics dicarboxyl that heat is sent to the first serosity heat exchanger from high-pressure steam
Calyx seu fructus physalis liquid.
Scheme 6
According to the method described in scheme 5, the pressure of wherein said high-pressure steam be about 50-150BarA,
Or about 75-125BarA or about 100BarA.
Scheme 7
According to the method described in scheme 5 or scheme 6, its mesohigh condensate produces also in step v)
And wherein step i) is further comprising the steps of:
Vi) heat is sent to the described thick aromatics the second serosity heat exchanger from described high pressure condensate
Dicarboxylic acids serosity, described second serosity heat exchanger is relative to the flow direction of described thick aromatic dicarboxylic acid serosity
It is arranged in the upstream of described first serosity heat exchanger.
Scheme 8
According to the method described in scheme 7, wherein in the flow direction relative to described thick aromatic dicarboxylic acid serosity
The upstream of described second serosity heat exchanger, described thick aromatic dicarboxylic acid serosity is heated at least
250℃。
Scheme 9
According to the method described in scheme 8, wherein in the flow direction relative to described thick aromatic dicarboxylic acid serosity
The upstream of described second serosity heat exchanger, described thick aromatic dicarboxylic acid serosity is heated at least
250 DEG C, and the most directly heat is sent to described thick aromatics dicarboxyl from high-pressure steam or high pressure condensate
Calyx seu fructus physalis liquid.
Scheme 10
According to the method described in any one in scheme 7-9, wherein step i) is further comprising the steps of:
Vii) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Described thick aromatic dicarboxylic acid serosity in 3rd serosity heat exchanger, described 3rd serosity heat exchanger phase
The flow direction for described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described second serosity heat exchanger.
Scheme 11
According to the method described in scheme 10, wherein step iii) include from described hydrogenation reactor
The aromatic dicarboxylic acid solution of described purification is sent to two or more crystallizers a series of.
Scheme 12
According to the method described in scheme 11, wherein step vii) include heat from from described series
The crystallizer discharge stream of the first crystallizer is sent to the described thick virtue in described 3rd serosity heat exchanger
Race's dicarboxylic acids serosity.
Scheme 13
According to the method described in scheme 12, wherein step iv) include heat from from described series
The crystallizer discharge stream of the later crystallization device in the second crystallizer or described series is sent to described water and steams
Current in gas maker are to generate steam.
Scheme 14
According to the method described in scheme 13, wherein step iv) include heat from from described series
The current that the crystallizer discharge stream of the second crystallizer is sent in described steam maker are to generate water
Steam.
Scheme 15
According to the method described in scheme 14, wherein step i) is further comprising the steps of:
Viii) heat is sent to the 4th from the crystallizer discharge stream from the second crystallizer described series
Described thick aromatic dicarboxylic acid serosity in serosity heat exchanger, described 4th serosity heat exchanger relative to
The flow direction of described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described 3rd serosity heat exchanger.
Scheme 16
A kind of method for adding hot gas stream in the method prepare aromatic dicarboxylic acid, described preparation virtue
The method of race's dicarboxylic acids include hydrocarbon precursor in organic solvent catalysis oxidation, described in add hot gas stream
Method comprises the following steps:
I) by generating steam according to the method described in any one in scheme 1-15；And
II) in the first gas heat-exchanger, heat is sent to described gas stream from described steam.
Scheme 17
According to the method described in scheme 16, wherein said gas stream is pressurization scrubber discharge gas stream.
Scheme 18
According to the method described in scheme 17, described method is further comprising the steps of:
III) described pressurization scrubber discharge gas stream heat being sent in the second gas heat-exchanger,
Described second gas heat-exchanger is arranged in relative to the flow direction of described pressurization scrubber discharge gas stream
The upstream of described first gas heat-exchanger.
Scheme 19
According to the method described in scheme 18, described method is further comprising the steps of:
IV) gas streaming is discharged by the described pressurization scrubber from described first gas heat-exchanger
To the 3rd gas heat-exchanger；
V) gas streaming is discharged by the described pressurization scrubber from described 3rd gas heat-exchanger
To catalytic burner；And
VI) catalytic burner exit gas is streamed to described 3rd gas heat-exchanger so that will
Heat is streamed to described pressurization scrubber discharge gas stream from described catalytic burner exit gas.
Scheme 20
According to the method described in any one in aforementioned schemes, wherein said aromatic dicarboxylic acid is to benzene two
Formic acid.
Scheme 21
A kind of equipment for generating steam in the method prepare aromatic dicarboxylic acid, described preparation virtue
The method of race's dicarboxylic acids includes the catalysis oxidation in organic solvent of hydrocarbon precursor, and described equipment includes:
A) the first serosity heat exchanger, described first serosity heat exchanger arrangement is for receiving thick aromatics dicarboxyl
Calyx seu fructus physalis liquid；
B) hydrogenation reactor, described hydrogenation reactor is configured to receive from described first serosity heat exchange
The thick aromatic dicarboxylic acid solution of device；
C) a series of one or more crystallizer, the one or more crystallizer is configured to receive
Aromatic dicarboxylic acid solution from the purification of described hydrogenation reactor；And
D) steam maker, described steam maker is configured to heat from from the one of described series
Individual or multiple crystallizer crystallizer discharge stream is sent to current to generate steam.
Scheme 22
According to the equipment described in scheme 21, the described steam wherein generated by steam maker d)
For middle setting-out steam or mesohigh steam.
Scheme 23
According to the equipment described in scheme 22, the described steam wherein generated by steam maker d)
For mesohigh steam.
Scheme 24
According to the equipment described in scheme 22 or scheme 23, the pressure of wherein said mesohigh steam is
About 10-50BarA or about 12.5-40barA or about 15-35BarA or about 17.5-30barA,
Or about 20BarA.
Scheme 25
According to the equipment described in any one in scheme 21-24, wherein said first serosity heat exchanger
It is configured to from high-pressure steam, heat is sent to described thick aromatic dicarboxylic acid serosity.
Scheme 26
According to the equipment described in scheme 25, the pressure of wherein said high-pressure steam is about 50-150
BarA or about 75-125BarA or about 100BarA.
Scheme 27
According to the equipment described in scheme 25 or scheme 26, described equipment also includes:
E) the second serosity heat exchanger, described second serosity heat exchanger arrangement is from by described height by heat
The high pressure condensate that setting-out steam generates is sent to described thick aromatic dicarboxylic acid serosity, and relative to institute
The flow direction stating thick aromatic dicarboxylic acid serosity is arranged in the upstream of described first serosity heat exchanger.
Scheme 28
According to the equipment described in scheme 26, wherein said equipment is configured to relative to described thick aromatics
The upstream of the described second serosity heat exchanger of the flow direction of dicarboxylic acids serosity, by described thick aromatic dicarboxylic acid
Serosity is heated at least 250 DEG C.
Scheme 29
According to the equipment described in scheme 28, wherein said equipment is configured to relative to described thick aromatics
The upstream of the described second serosity heat exchanger of the flow direction of dicarboxylic acids serosity, by described thick aromatic dicarboxylic acid
Serosity is heated at least 250 DEG C, and the most directly heat is sent to from high-pressure steam or high pressure condensate
Described thick aromatic dicarboxylic acid serosity.
Scheme 30
According to the equipment described in any one in scheme 27-29, described equipment also includes:
F) the 3rd serosity heat exchanger, described 3rd serosity heat exchanger arrangement is from from described by heat
The crystallizer discharge stream of one or more crystallizers of series is sent to described thick aromatic dicarboxylic acid serosity,
And it is arranged in described second serosity heat exchange relative to the flow direction of described thick aromatic dicarboxylic acid serosity
The upstream of device.
Scheme 31
According to the equipment described in scheme 30, wherein said equipment includes a series of plural knot
Brilliant device.
Scheme 32
According to the equipment described in scheme 31, wherein said 3rd serosity heat exchanger arrangement be by heat from
Crystallizer discharge stream from the first crystallizer in described series is sent to described thick aromatic dicarboxylic acid
Serosity.
Scheme 33
According to the equipment described in scheme 32, wherein said steam maker be configured to by heat from from
The crystallizer discharge of the second crystallizer in described series or the later crystallization device in described series is spread
Deliver to described current to generate steam.
Scheme 34
According to the equipment described in scheme 33, wherein said steam maker be configured to by heat from from
The crystallizer discharge stream of the second crystallizer in described series is sent to described current to generate steam.
Scheme 35
According to the equipment described in scheme 34, described equipment also includes:
G) the 4th serosity heat exchanger, described 4th serosity heat exchanger arrangement is from from described by heat
The crystallizer discharge stream of the second crystallizer in series is sent to described thick aromatic dicarboxylic acid serosity, and
It is arranged in described 3rd serosity heat exchanger relative to the flow direction of described thick aromatic dicarboxylic acid serosity
Upstream.
Scheme 36
A kind of equipment for adding hot gas stream in the method prepare aromatic dicarboxylic acid, described preparation virtue
The method of race's dicarboxylic acids includes the catalysis oxidation in organic solvent of hydrocarbon precursor, and described equipment includes:
A) according to the equipment for generating steam described in any one in scheme 21-35；And
B) the first gas heat-exchanger, described first gas heat-exchanger is configured to steam heat from described water
Gas is sent to described gas stream.
Scheme 37
According to the equipment described in scheme 36, wherein said gas stream is pressurization scrubber discharge gas stream.
Scheme 38
According to the equipment described in scheme 37, described equipment also includes:
C) the second gas heat-exchanger, described second gas heat-exchanger is configured to be sent to heat described
Gas stream, and described second gas heat-exchanger is arranged in described relative to the flow direction of described gas stream
The upstream of the first gas heat-exchanger.
Scheme 39
According to the equipment described in scheme 38, described equipment also includes:
D) the 3rd gas heat-exchanger, described 3rd gas heat-exchanger is configured to receive from described the
The described pressurization scrubber discharge gas stream of one gas heat-exchanger；And
E) catalytic burner, described catalytic burner is configured to receive from described 3rd air heat exchange
The described pressurization scrubber discharge gas stream of device,
Wherein said 3rd gas heat-exchanger is additionally configured to receive catalytic burner exit gas stream and by heat
It is streamed to described pressurization scrubber discharge gas stream from described catalytic burner exit gas.
Scheme 40
According to the equipment described in any one in scheme 21-39, wherein said aromatic dicarboxylic acid is to benzene
Dioctyl phthalate.
Scheme 41
A kind of method for preparing aromatic dicarboxylic acid, the described method preparing aromatic dicarboxylic acid includes hydrocarbon
Precursor catalysis oxidation in organic solvent, the described method preparing aromatic dicarboxylic acid comprises the following steps:
I) aoxidize described hydrocarbon precursor in organic solvent to provide thick virtue in the presence of metallic catalyst
Race's dicarboxylic acids serosity；
Wherein said method is further comprising the steps of:
Ii) described thick aromatic dicarboxylic acid serosity is heated to form thick aromatic dicarboxylic acid solution；
Iii) described thick aromatic dicarboxylic acid solution is sent to hydrogenation reactor；
Iv) the aromatic dicarboxylic acid solution of purification is sent to a series of one from described hydrogenation reactor
Or multiple crystallizer；With
V) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current in steam maker are to generate steam.
Scheme 42
According to the method described in scheme 41, said method comprising the steps of:
The gas stream that heat is sent to the first gas heat-exchanger from described steam.
Additionally, in some embodiments, the disclosure also includes following additional aspects.
Additional aspects 1
A kind of equipment generating steam, described equipment makes in the system for preparing aromatic dicarboxylic acid
With, described equipment includes:
A) the first serosity heat exchanger of thick aromatic dicarboxylic acid serosity is received；
B) hydrogenation of the thick aromatic dicarboxylic acid solution from described first serosity heat exchanger is received
Device；
C) receive from described hydrogenation reactor purification aromatic dicarboxylic acid solution a series of one
Individual or multiple crystallizers；And
D) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current are to generate the steam maker of steam.
Additional aspects 2
According to the equipment described in additional aspects 1, wherein said first serosity heat exchanger is connected to high pressure
Source of water vapor.
Additional aspects 3
According to the equipment described in additional aspects 1, described equipment also includes
E) heat is sent to described thick aromatics two from the high pressure condensate generated by described high-pressure steam
Second serosity heat exchanger of carboxylic acid slurry, and described second serosity heat exchanger relative to described slightly
The flow direction of aromatic dicarboxylic acid serosity is arranged in the upstream of described first serosity heat exchanger.
Additional aspects 4
According to the equipment described in additional aspects 1, described equipment also includes
F) heat is sent to institute from the crystallizer discharge stream of the one or more crystallizers from described series
State the 3rd serosity heat exchanger of thick aromatic dicarboxylic acid serosity, and described 3rd serosity heat exchanger phase
The flow direction for described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described second serosity heat exchanger.
Additional aspects 5
According to the equipment described in additional aspects 4, wherein said equipment includes a series of plural
Crystallizer.
Additional aspects 6
According to the equipment described in additional aspects 5, wherein said 3rd serosity heat exchanger is connected to described
The floss hole of the first crystallizer in series.
Additional aspects 7
According to the equipment described in additional aspects 6, wherein said steam maker is connected to described series
In the floss hole of the second crystallizer or the floss hole of later crystallization device in described series.
Additional aspects 8
According to the equipment described in additional aspects 7, during wherein steam maker is connected to described series
The floss hole of the second crystallizer.
Additional aspects 9
According to the equipment described in additional aspects 8, described equipment includes
G) heat is sent to described from the crystallizer discharge stream from the second crystallizer described series
4th serosity heat exchanger of thick aromatic dicarboxylic acid serosity, and described 4th serosity heat exchanger is relative
The flow direction in described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described 3rd serosity heat exchanger.
Additional aspects 10
A kind of equipment adding hot gas stream, described equipment makes in the system for preparing aromatic dicarboxylic acid
With, described equipment includes:
A) according to the equipment for generating steam described in any one in additional aspects 1-9；And
B) heat is sent to from described steam the first gas heat-exchanger of described gas stream.
Additional aspects 11
According to the equipment described in additional aspects 10, described equipment also includes
C) heat is sent to the second gas heat-exchanger of described gas stream, and described second air heat
Exchanger is arranged in the upstream of described first gas heat-exchanger relative to the flow direction of described gas stream.
Additional aspects 12
According to the equipment described in additional aspects 11, described equipment also includes processing adding of described gas stream
Pressure scrubber.
Additional aspects 13
According to the equipment described in additional aspects 12, wherein said pressurization scrubber is connected to described second
Gas heat-exchanger.
Additional aspects 14
According to the equipment described in additional aspects 13, described equipment also includes
D) the 3rd of the pressurization scrubber discharge gas stream from described first gas heat-exchanger is received
Gas heat-exchanger；And
E) catalysis of the pressurization scrubber discharge gas stream from described 3rd gas heat-exchanger is received
Burner,
Wherein said 3rd gas heat-exchanger also receives catalytic burner exit gas stream.
Additional aspects 15
According to the equipment described in additional aspects 1, wherein said steam maker is shell-and-tube heat exchange
Device.
Additional aspects 16
A kind of system for preparing aromatic dicarboxylic acid, described system include according to additional aspects 1 to
The equipment described in any one in 15.
Additional aspects 17
A kind of system for preparing aromatic dicarboxylic acid, described system includes
Oxidation panel,
Crystallized region, described crystallized region includes one or more crystallizer；
Process the distilling period of the discharge gas from described oxidation panel；
Condensation segment, described condensation segment is connected to described distilling period；
Overhead gas in autocondensation in future section discharge to before atmospheric environment to adding that it processes
Pressure scrubber；With
According to the equipment described in any one in additional aspects 1 to 15.
Claims (42)
1. for the method generating steam in the method prepare aromatic dicarboxylic acid, described system
The method of standby aromatic dicarboxylic acid includes the catalysis oxidation in organic solvent of hydrocarbon precursor, and described generation water steams
The method of gas comprises the following steps:
I) thick aromatic dicarboxylic acid serosity is heated to form thick aromatic dicarboxylic acid solution；
Ii) described thick aromatic dicarboxylic acid solution is sent to hydrogenation reactor；
Iii) the aromatic dicarboxylic acid solution of purification is sent to a series of one from described hydrogenation reactor
Or multiple crystallizer；And
Iv) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current in steam maker are to generate steam.
Method the most according to claim 1, wherein in step iv) in the steam that generates be
Setting-out steam or mesohigh steam.
Method the most according to claim 2, wherein in step iv) in the steam that generates be
High-pressure steam.
4., according to the method described in claim 2 or claim 3, wherein said mesohigh water steams
The pressure of gas is about 10-50BarA or about 12.5-40barA or about 15-35BarA or about
17.5-30barA or about 20BarA.
5., according to the method described in any one in claim 1-4, wherein step i) includes following step
Rapid:
V) the described thick aromatics dicarboxyl that heat is sent to the first serosity heat exchanger from high-pressure steam
Calyx seu fructus physalis liquid.
Method the most according to claim 5, the pressure of wherein said high-pressure steam is about
50-150BarA or about 75-125BarA or about 100BarA.
7., according to the method described in claim 5 or claim 6, its mesohigh condensate is in step
Rapid v) middle generation and wherein step i) are further comprising the steps of:
Vi) heat is sent to the described thick aromatics the second serosity heat exchanger from described high pressure condensate
Dicarboxylic acids serosity, described second serosity heat exchanger is relative to the flow direction of described thick aromatic dicarboxylic acid serosity
It is arranged in the upstream of described first serosity heat exchanger.
Method the most according to claim 7, is wherein starching relative to described thick aromatic dicarboxylic acid
The upstream of the described second serosity heat exchanger of the flow direction of liquid, heats described thick aromatic dicarboxylic acid serosity
To at least 250 DEG C.
Method the most according to claim 8, is wherein starching relative to described thick aromatic dicarboxylic acid
The upstream of the described second serosity heat exchanger of the flow direction of liquid, heats described thick aromatic dicarboxylic acid serosity
To at least 250 DEG C, and the most directly heat is sent to described thick virtue from high-pressure steam or high pressure condensate
Race's dicarboxylic acids serosity.
10. according to the method described in any one in claim 7-9, wherein step i) also include with
Lower step:
Vii) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Described thick aromatic dicarboxylic acid serosity in 3rd serosity heat exchanger, described 3rd serosity heat exchanger phase
The flow direction for described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described second serosity heat exchanger.
11. method according to claim 10, wherein steps iii) include from described hydrogenation
The aromatic dicarboxylic acid solution of the described purification of reactor is sent to two or more crystallizations a series of
Device.
12. method according to claim 11, wherein steps vii) include heat from from described
The crystallizer discharge stream of the first crystallizer in series is sent in described 3rd serosity heat exchanger
Described thick aromatic dicarboxylic acid serosity.
13. method according to claim 12, wherein steps iv) include heat from from described
The crystallizer discharge stream of the second crystallizer in series or the later crystallization device in described series is sent to
Current in described steam maker are to generate steam.
14. method according to claim 13, wherein steps iv) include heat from from described
The crystallizer discharge stream of the second crystallizer in series is sent to the current in described steam maker
To generate steam.
15. methods according to claim 14, wherein step i) is further comprising the steps of:
Viii) heat is sent to the 4th from the crystallizer discharge stream from the second crystallizer described series
Described thick aromatic dicarboxylic acid serosity in serosity heat exchanger, described 4th serosity heat exchanger relative to
The flow direction of described thick aromatic dicarboxylic acid serosity is arranged in the upstream of described 3rd serosity heat exchanger.
16. 1 kinds for the method adding hot gas stream in the method prepare aromatic dicarboxylic acid, described system
The method of standby aromatic dicarboxylic acid includes the catalysis oxidation in organic solvent of hydrocarbon precursor, described in add hot gas
The method of stream comprises the following steps:
I) by generating steam according to the method described in any one in claim 1-15；And
II) in the first gas heat-exchanger, heat is sent to described gas stream from described steam.
17. methods according to claim 16, wherein said gas stream is pressurization scrubber row
Venting body stream.
18. methods according to claim 17, described method is further comprising the steps of:
III) described pressurization scrubber discharge gas stream heat being sent in the second gas heat-exchanger,
Described second gas heat-exchanger is arranged in relative to the flow direction of described pressurization scrubber discharge gas stream
The upstream of described first gas heat-exchanger.
19. methods according to claim 18, described method is further comprising the steps of:
IV) gas streaming is discharged by the described pressurization scrubber from described first gas heat-exchanger
To the 3rd gas heat-exchanger；
V) gas streaming is discharged by the described pressurization scrubber from described 3rd gas heat-exchanger
To catalytic burner；And
VI) catalytic burner exit gas is streamed to described 3rd gas heat-exchanger so that will
Heat is streamed to described pressurization scrubber discharge gas stream from described catalytic burner exit gas.
20. according to the method described in any one in aforementioned claim, wherein said aromatic dicarboxylic acid
For p-phthalic acid.
21. 1 kinds for generating the equipment of steam, described system in the method prepare aromatic dicarboxylic acid
The method of standby aromatic dicarboxylic acid includes the catalysis oxidation in organic solvent of hydrocarbon precursor, and described equipment includes:
A) the first serosity heat exchanger, described first serosity heat exchanger arrangement is for receiving thick aromatics dicarboxyl
Calyx seu fructus physalis liquid；
B) hydrogenation reactor, described hydrogenation reactor is configured to receive from described first serosity heat exchange
The thick aromatic dicarboxylic acid solution of device；
C) a series of one or more crystallizer, the one or more crystallizer is configured to receive
Aromatic dicarboxylic acid solution from the purification of described hydrogenation reactor；And
D) steam maker, described steam maker is configured to heat from from the one of described series
Individual or multiple crystallizer crystallizer discharge stream is sent to current to generate steam.
22. equipment according to claim 21, the institute wherein generated by steam maker d)
Stating steam is middle setting-out steam or mesohigh steam.
23. equipment according to claim 22, the institute wherein generated by steam maker d)
Stating steam is mesohigh steam.
24. according to the equipment described in claim 22 or claim 23, wherein said mesohigh water
The pressure of steam is about 10-50BarA or about 12.5-40barA or about 15-35BarA or about
17.5-30barA or about 20BarA.
25. according to the equipment described in any one in claim 21-24, wherein said first serosity
Heat exchanger arrangement is for be sent to described thick aromatic dicarboxylic acid serosity by heat from high-pressure steam.
26. equipment according to claim 25, the pressure of wherein said high-pressure steam is about
50-150BarA or about 75-125BarA or about 100BarA.
27. also include according to the equipment described in claim 25 or claim 26, described equipment:
E) the second serosity heat exchanger, described second serosity heat exchanger arrangement is from by described height by heat
The high pressure condensate that setting-out steam generates is sent to described thick aromatic dicarboxylic acid serosity, and relative to institute
The flow direction stating thick aromatic dicarboxylic acid serosity is arranged in the upstream of described first serosity heat exchanger.
28. equipment according to claim 26, wherein said equipment is configured to relative to institute
State the upstream of the described second serosity heat exchanger of the flow direction of thick aromatic dicarboxylic acid serosity, by described thick virtue
Race's dicarboxylic acids serosity is heated at least 250 DEG C.
29. equipment according to claim 28, wherein said equipment is configured to relative to institute
State the upstream of the described second serosity heat exchanger of the flow direction of thick aromatic dicarboxylic acid serosity, by described thick virtue
Race's dicarboxylic acids serosity is heated at least 250 DEG C, and the most directly heat is condensed from high-pressure steam or high pressure
Thing is sent to described thick aromatic dicarboxylic acid serosity.
30. also include according to the equipment described in any one in claim 27-29, described equipment:
F) the 3rd serosity heat exchanger, described 3rd serosity heat exchanger arrangement is from from described by heat
The crystallizer discharge stream of one or more crystallizers of series is sent to described thick aromatic dicarboxylic acid serosity,
And it is arranged in described second serosity heat exchange relative to the flow direction of described thick aromatic dicarboxylic acid serosity
The upstream of device.
31. equipment according to claim 30, wherein said equipment includes a series of two
Above crystallizer.
32. equipment according to claim 31, wherein said 3rd serosity heat exchanger arrangement
For heat is sent to described thick virtue from the crystallizer discharge stream from the first crystallizer described series
Race's dicarboxylic acids serosity.
33. equipment according to claim 32, wherein said steam maker be configured to by
Heat is from the crystallizer from the second crystallizer described series or the later crystallization device in described series
Discharge stream is sent to described current to generate steam.
34. equipment according to claim 33, wherein said steam maker be configured to by
Heat is sent to described current with life from the crystallizer discharge stream from the second crystallizer described series
Become steam.
35. equipment according to claim 34, described equipment also includes:
G) the 4th serosity heat exchanger, described 4th serosity heat exchanger arrangement is from from described by heat
The crystallizer discharge stream of the second crystallizer in series is sent to described thick aromatic dicarboxylic acid serosity, and
It is arranged in described 3rd serosity heat exchanger relative to the flow direction of described thick aromatic dicarboxylic acid serosity
Upstream.
36. 1 kinds for adding the equipment of hot gas stream, described system in the method prepare aromatic dicarboxylic acid
The method of standby aromatic dicarboxylic acid includes the catalysis oxidation in organic solvent of hydrocarbon precursor, and described equipment includes:
A) according to the equipment for generating steam described in any one in claim 21-35；With
And
B) the first gas heat-exchanger, described first gas heat-exchanger is configured to steam heat from described water
Gas is sent to described gas stream.
37. equipment according to claim 36, wherein said gas stream is pressurization scrubber row
Venting body stream.
38. also include according to the equipment described in claim 37, described equipment:
C) the second gas heat-exchanger, described second gas heat-exchanger is configured to be sent to heat described
Gas stream, and described second gas heat-exchanger is arranged in described relative to the flow direction of described gas stream
The upstream of the first gas heat-exchanger.
39. also include according to the equipment described in claim 38, described equipment:
D) the 3rd gas heat-exchanger, described 3rd gas heat-exchanger is configured to receive from described the
The described pressurization scrubber discharge gas stream of one gas heat-exchanger；And
E) catalytic burner, described catalytic burner is configured to receive from described 3rd air heat exchange
The described pressurization scrubber discharge gas stream of device,
Wherein said 3rd gas heat-exchanger is additionally configured to receive catalytic burner exit gas stream and by heat
It is streamed to described pressurization scrubber discharge gas stream from described catalytic burner exit gas.
40. according to the equipment described in any one in claim 21-39, wherein said aromatics dicarboxyl
Acid is p-phthalic acid.
41. 1 kinds for the method preparing aromatic dicarboxylic acid, the described method bag preparing aromatic dicarboxylic acid
Including the catalysis oxidation in organic solvent of hydrocarbon precursor, the described method preparing aromatic dicarboxylic acid includes following
Step:
I) aoxidize described hydrocarbon precursor in organic solvent to provide thick virtue in the presence of metallic catalyst
Race's dicarboxylic acids serosity；
Wherein said method is further comprising the steps of:
Ii) described thick aromatic dicarboxylic acid serosity is heated to form thick aromatic dicarboxylic acid solution；
Iii) described thick aromatic dicarboxylic acid solution is sent to hydrogenation reactor；
Iv) the aromatic dicarboxylic acid solution of purification is sent to a series of one from described hydrogenation reactor
Or multiple crystallizer；With
V) heat is sent to from the crystallizer discharge stream of the one or more crystallizers from described series
Current in steam maker are to generate steam.
42. methods according to claim 41, said method comprising the steps of:
The gas stream that heat is sent to the first gas heat-exchanger from described steam.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110202650.4A CN112979460A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
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| GB1417636.6 | 2014-10-06 | ||
| GBGB1417636.6A GB201417636D0 (en) | 2014-10-06 | 2014-10-06 | Production of an aromatic dicarboxylic acid |
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| CN201520108168.4U Active CN204714728U (en) | 2014-10-06 | 2015-02-13 | Generate the equipment of water vapour, the equipment of heated air stream and the system for the preparation of aromatic dicarboxylic acid |
| CN201510079766.8A Pending CN105985237A (en) | 2014-10-06 | 2015-02-13 | Production of an aromatic dicarboxylic acid |
| CN202110202650.4A Pending CN112979460A (en) | 2014-10-06 | 2015-02-13 | Preparation of aromatic dicarboxylic acids |
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| CN (3) | CN204714728U (en) |
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| WO (1) | WO2016055456A2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110997610A (en) * | 2017-08-01 | 2020-04-10 | Bp北美公司 | Method for preheating boiler feed water in manufacture of purified aromatic carboxylic acid |
| CN112341325A (en) * | 2020-12-02 | 2021-02-09 | 台化兴业(宁波)有限公司 | Energy recovery device and method for aromatic dicarboxylic acid production process |
| CN112979460A (en) * | 2014-10-06 | 2021-06-18 | 英威达纺织（英国）有限公司 | Preparation of aromatic dicarboxylic acids |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD289891A7 (en) * | 1989-03-22 | 1991-05-16 | Petrolchemie Und Kraftstoffe Ag,De | PROCESS FOR CLEANING TEREPHTHALIC ACID |
| CN101045683A (en) * | 2006-03-27 | 2007-10-03 | 三井化学株式会社 | Method of preparing high-purity terephthalic acid |
| CN101637699A (en) * | 2008-08-02 | 2010-02-03 | 中国石油化工股份有限公司 | Method for purifying waste gas of pure terephthalic acid producing device |
Family Cites Families (1)
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|---|---|---|---|---|
| GB201417636D0 (en) * | 2014-10-06 | 2014-11-19 | Invista Tech Sarl | Production of an aromatic dicarboxylic acid |
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- 2014-10-06 GB GBGB1417636.6A patent/GB201417636D0/en not_active Ceased
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2015
- 2015-02-13 CN CN201520108168.4U patent/CN204714728U/en active Active
- 2015-02-13 CN CN201510079766.8A patent/CN105985237A/en active Pending
- 2015-02-13 CN CN202110202650.4A patent/CN112979460A/en active Pending
- 2015-10-06 WO PCT/EP2015/073021 patent/WO2016055456A2/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD289891A7 (en) * | 1989-03-22 | 1991-05-16 | Petrolchemie Und Kraftstoffe Ag,De | PROCESS FOR CLEANING TEREPHTHALIC ACID |
| CN101045683A (en) * | 2006-03-27 | 2007-10-03 | 三井化学株式会社 | Method of preparing high-purity terephthalic acid |
| CN101637699A (en) * | 2008-08-02 | 2010-02-03 | 中国石油化工股份有限公司 | Method for purifying waste gas of pure terephthalic acid producing device |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979460A (en) * | 2014-10-06 | 2021-06-18 | 英威达纺织（英国）有限公司 | Preparation of aromatic dicarboxylic acids |
| CN110997610A (en) * | 2017-08-01 | 2020-04-10 | Bp北美公司 | Method for preheating boiler feed water in manufacture of purified aromatic carboxylic acid |
| CN112341325A (en) * | 2020-12-02 | 2021-02-09 | 台化兴业(宁波)有限公司 | Energy recovery device and method for aromatic dicarboxylic acid production process |
Also Published As
| Publication number | Publication date |
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| WO2016055456A2 (en) | 2016-04-14 |
| CN112979460A (en) | 2021-06-18 |
| GB201417636D0 (en) | 2014-11-19 |
| WO2016055456A3 (en) | 2016-06-02 |
| CN204714728U (en) | 2015-10-21 |
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