WO2010064006A1 - Systèmes et procédés pour la gestion de régimes transitoires d'un réacteur - Google Patents

Systèmes et procédés pour la gestion de régimes transitoires d'un réacteur Download PDF

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Publication number
WO2010064006A1
WO2010064006A1 PCT/GB2009/002804 GB2009002804W WO2010064006A1 WO 2010064006 A1 WO2010064006 A1 WO 2010064006A1 GB 2009002804 W GB2009002804 W GB 2009002804W WO 2010064006 A1 WO2010064006 A1 WO 2010064006A1
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WIPO (PCT)
Prior art keywords
machine train
expander
steam
reactor
oxidation reactor
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PCT/GB2009/002804
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English (en)
Inventor
Gillian Kerr
Robert John O'brien
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Invista Technologies S.A.R.L.
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Publication date
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Priority to CN200980148568.5A priority Critical patent/CN102239000B/zh
Publication of WO2010064006A1 publication Critical patent/WO2010064006A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00006—Large-scale industrial plants

Definitions

  • aromatic carboxylic acids such as terephthalic acid (TA) typically involves the liquid-phase oxidation of an aromatic feedstock compound, such as paraxylene, using molecular oxygen in a solvent, usually in the presence of a catalyst that incorporates a promoter.
  • an aromatic feedstock compound such as paraxylene
  • a catalyst that incorporates a promoter.
  • the solvent, molecular oxygen, feedstock, and catalyst are continuously fed into an oxidation reactor at an elevated temperature and pressure.
  • Feedstock oxidation within the reactor produces a high- pressure gaseous stream or "off-gas" that typically comprises nitrogen, unreacted oxygen, carbon dioxide, carbon monoxide and, where bromine is used as a promoter, methyl bromide. Because the reaction is exothermic, the solvent is often allowed to vaporize to control the reaction temperature. Therefore, the off-gas can further comprise vaporized solvent.
  • the off-gas from the reactor contains a significant amount of energy, which can be recovered to reduce the total energy consumed during production and at least partially offset the cost of obtaining the high temperatures and pressures required by the oxidation reactor.
  • the off-gas is directed to an expander that drives a compressor, which feeds pressurized air to the reactor. Steam raised while condensing the gaseous stream that is not required elsewhere can be directed to a turbine that is also used to drive the compressor.
  • transient conditions occur and air feed to the reactor must be cut, the off-gas from the reactor quickly reduces to zero and steam is no longer raised by the condensers for the turbine.
  • the machine train which includes the turbine, the expander, and the compressor, must either be shut down or supplemental energy must be applied to keep the machine train online. Because of the time and cost associated with bringing the machine train back online after shut down, it is generally preferable to keep the machine train online while the issue that caused the transient is being resolved. Unfortunately, the costs of keeping the machine train online are undesirably high due to the substantial amounts of supplemental energy, in the form of high pressure steam and/or electricity from an auxiliary source, that are required to keep the machine train running at its normal operating speed.
  • FIG. 1 is a schematic view of an embodiment of a system for producing an aromatic carboxylic acid.
  • an axial or radial single-shaft compressor can be used in the machine train of an aromatic carboxylic acid production plant that, unlike the integrally-geared compressors typically used in such plants, can be safely operated over a wide range of speeds.
  • the machine train speed can be reduced to the point at which the supplemental steam and/or electric power needed to operate the machine train while the reactor is offline is reduced to a third of what would normally be required.
  • the use of a single-shaft compressor and the reduced machine train operating speeds it facilitates enables the use of smaller boilers within the plant, thereby potentially reducing plant equipment costs.
  • the plant incorporates an air bypass route that extends from the compressor to the expander.
  • a control system opens the bypass route to deliver compressed air to the expander, and deliberately reduces the train speed to a setpoint in the range of approximately 70% to 95% of normal operating speed.
  • the particular setpoint selected depends on machine configurations for both thermodynamic characteristics and mechanical requirements, such as torsional excitation, impeller resonance, blade pass interference, and lateral critical speeds. Regardless, because the expander is maintained at an elevated temperature due to the redirection of compressed air from the compressor, the machine train can be quickly ramped back up to normal operating speed once the transient condition has been resolved.
  • FIG. 1 illustrated is an example system 10 for producing aromatic carboxylic acid by the exothermic, liquid-phase oxidation of an aromatic feedstock compound.
  • the system 10 comprises part of a larger aromatic carboxylic acid production plant including other components of which are not illustrated in FIG. 1.
  • the system 10 comprises a reaction system 12 that includes an oxidation reactor 14 in which the aromatic feedstock can be oxidized to produce the aromatic carboxylic acid. More particularly, an aromatic carboxylic acid can be produced within the reactor 14 through the high pressure, exothermic oxidation of a suitable aromatic feedstock compound in a liquid-phase reaction using an oxidant, an oxidation solvent, a catalyst, and a promoter.
  • the aromatic feedstock compound used can be any aromatic compound that has oxidizable substituents that can be oxidized to a carboxylic acid group.
  • the oxidizable substituent can be an alkyl group such as a methyl, ethyl, or isopropyl group.
  • the substituent can also be a partially-oxidized alkyl group, such as an alcohol group, aldehyde group, or ketone group.
  • the aromatic portion of the aromatic feedstock compound can be a benzene nucleus or it can be bi- or polycyclic, for example a naphthalene nucleus.
  • the number of oxidizable substituents on the aromatic portion of the aromatic feedstock compound can be equal to the number of sites available on the aromatic portion of the aromatic feedstock compound, but is generally fewer, for example 1 to about 4, suitably 2 or 3.
  • suitable aromatic feedstock compounds include toluene, ethylbenzene, oxylene, metaxylene, paraxylene, 1-formyl-4-methylbenzene, 1-hydroxymethyl-4- methylbenzene, 1 ,2,4-trimethylbenzene, 1-formyl-2,4-dimethylbenzene, 1 ,2,4,5- tetramethylbenzene, alkyl, hydroxymethyl, formyl, and acyl substituted naphthalene compounds such as 2,6- and 2,7-dimethylnaphthalene, 2-acyl-6-methylnaphthalene, 2-formyl-6-methylnaphthalene, 2-methyl-6-ethylnaphthalene, 2,6-diethylnaphthalene,
  • the aromatic feedback compound is paraxylene (PX) and it is used to produce terephthalic acid (TA).
  • TA terephthalic acid
  • Molecular oxygen can be used as the oxidant.
  • air which can be oxygen enriched or depleted, is a suitable source of molecular oxygen.
  • the oxygen-containing gas fed to the oxidation reactor 14 provides an exhaust gas-vapor mixture containing from approximately 0.5 to approximately 8 volume percent oxygen (measured on a solvent-free basis).
  • a feed rate of the oxygen-containing gas sufficient to provide oxygen in the amount of from approximately 1.5 to approximately 2.8 moles per methyl group will provide approximately 0.5 to 8 volume percent of oxygen (measured on a solvent-free basis) in the overhead gas-vapor mixture.
  • the oxidation solvent can be a low molecular weight aliphatic monocarboxylic acid having approximately 2 to 6 carbon atoms, or mixtures thereof with water.
  • the solvent comprises an acetic acid or a mixture of an acetic acid and water.
  • Suitable catalysts include those heavy metals having an atomic number of approximately 21 to about 82 such as a mixture of cobalt and manganese, and suitable promoters include bromine promoter compounds such as hydrogen bromide, molecular bromine, and sodium bromide.
  • the catalyst/promoter employed in producing crude terephthalic acid can, for example, comprise cobalt, manganese, and bromine components, and can additionally comprise accelerators.
  • the ratio of cobalt (calculated as elemental cobalt) in the cobalt component of the catalyst-to- paraxylene in the liquid-phase oxidation can be in the range of about approximately 0.2 to 10 milligram atoms (mga) per gram mole of paraxylene.
  • the ratio of manganese (calculated as elemental manganese) in the manganese component of the catalyst-to-cobalt (calculated as elemental cobalt) in the cobalt component of the catalyst in the liquid-phase oxidation can be in the range of about approximately 0.2 to 10 mga per mga of cobalt.
  • the weight ratio of bromine (calculated as elemental bromine) in the bromine component of the catalyst-to-total cobalt and manganese (calculated as elemental cobalt and elemental manganese) in the cobalt and manganese components of the catalyst in the liquid-phase oxidation can be in the range of approximately 0.2 to 1.5 mga per mga of total cobalt and manganese.
  • Each of the cobalt and manganese components can be provided in any of its known ionic or combined forms that provide soluble forms of cobalt, manganese, and bromine in the solvent in the oxidation reactor 14.
  • the solvent is an acetic acid medium
  • cobalt and/or manganese carbonate, acetate tetrahydrate, and/or bromine can be employed.
  • the 0.2:1.0 to 1.5:1.0 bromine-to-total cobalt and manganese milligram atom ratio can be provided by a suitable source of bromine.
  • Such bromine sources can include elemental bromine (Br 2 ), ionic bromine ⁇ for example HBr, NaBr, KBr, NH 4 Br, etc.), or organic bromides that are known to provide bromide ions at the operating temperature of the oxidation (e.g., benzylbromide, mono- and di-bromoacetic acid, bromoacetyl bromide, tetrabromoethane, ethylene- di-bromide, etc.).
  • the total bromine in molecular bromine and ionic bromide is used to determine satisfaction of the elemental bromine-to-total cobalt and manganese milligram atom ratio of 0.2:1.0 to 1.5:1.0.
  • the bromine ion released from the organic bromides at the oxidation operating conditions can be readily determined by known analytical means.
  • the minimum pressure at which the oxidation reactor 14 is maintained is typically that pressure that will maintain a substantial liquid phase of the paraxylene and the solvent.
  • suitable reaction gauge pressures in the oxidation reactor 14 can be in the range of approximately 0 kg/cm 2 to 35 kg/cm 2 , and typically are in the range of approximately 10 kg/cm 2 to 20 kg/cm 2 .
  • the temperature range within the oxidation reactor can be, for example, approximately 120 0 C to 250 0 C.
  • the solvent residence time in the reactor 14 can be approximately 20 to 150 minutes, for example approximately 30 to 120 minutes.
  • the oxidation reactor 14 typically comprises a vessel that is constructed of or lined with a corrosion-resistant material, such as titanium or glass. Because the oxidation reaction is conducted at an elevated pressure, the reactor 14 is constructed to withstand the high pressures used for the oxidation reaction. In addition, the reactor 14 can be equipped with one or more mechanical agitators (not shown). Crude terephthalic acid produced by the oxidation reaction leaves the reactor 14 along a outlet line 16 in the form of an oxidation reaction slurry that comprises a mixture of crude terephthalic acid, water, acetic acid, catalyst metals, oxidation reaction intermediates, and reaction byproducts. The slurry can then be processed using a variety of procedures and equipment (not shown) to produce purified terephthalic acid.
  • a corrosion-resistant material such as titanium or glass.
  • the off-gas can be used to raise various pressures of steam that can, for example, be used to drive and/or heat other components of the system 10.
  • the off-gas exits the oxidation reactor 14 and flows through a gas line 18 to a series of condensers 20, 22, and 24, which condense the off-gas and raise steam.
  • the first condenser 20 can produce low pressure steam at approximately 145°C and approximately 4.5 bar
  • the second condenser 22 can produce extra-low pressure steam at approximately 130 0 C and approximately 3 bar
  • the condenser 24 can produce very-low pressure steam at approximately 100°C and approximately 1 bar.
  • the steam from the first condenser 20 flows along steam lines 26 and 28 to various low pressure steam users within the plant.
  • Examples of such users include reboilers and driers.
  • Steam from the second condenser 22 can flow along steam line 30, through control valve 32, and into a turbine 34 that is coupled to an electric generator 36 with a shaft 38. Therefore, steam raised using the second condenser 22 can be used to generate electricity, which can be used to drive various equipment of the plant.
  • a further steam line 40 is connected to the exit of the turbine 34 and delivers the steam to a heat exchanger 42, which condenses the steam into condensate that is output along condensate line 44.
  • a further steam line 50 also having a control valve 52 joins steam lines 26 and 30 to facilitate the delivery of steam from line 26 to line 30 for the purpose of driving the turbine 34.
  • a steam line 54 having a control valve 56 extends from the steam line 26 to a further turbine 58 described below.
  • Steam from the condenser 24 travels along a steam line 60 and is split into two paths, a first path 62 having a control valve 64 and leading to the turbine 58, and a second path 66 having a dump valve 68 and leading to a heat exchanger 70, which in an emergency condenses the steam into condensate that is output along condensate line 72.
  • Exhaust steam from turbine 58 is passed to the heat exchanger 70, which condenses the steam into condensate that is output along condensate line 72.
  • the system 10 includes a control valve 76 that couples the steam line 26 to a steam line 78 along which auxiliary high pressure (HP) steam, for instance produced by one or more small package boilers of the plant (not shown), can be input into the system.
  • HP high pressure
  • that steam can be provided to the turbine 58 during reactor transients.
  • the turbine 58 comprises one component of a machine train that also includes an air compressor 80 and an expander 82.
  • the turbine 58 is coupled to the air compressor 80 with a coupling 84
  • the expander 82 is coupled to the compressor with a coupling 86.
  • Both the turbine 58 and the expander 82 are used to drive the compressor 80, which draws in air along inlet line 88 and produces pressured air that can be supplied to the oxidation reactor 14 along air line 90.
  • the compressor 80 is an axial and/or radial single-shaft compressor, occasionally referred to as a "between-bearing" compressor, instead of a integrally- geared compressor typically used in TA plants, which typically comprise multiple shafts that operate at different speeds.
  • the compressor 80 supplies air to the reactor 14 at a temperature of approximately 150 0 C to 250°C and a pressure of approximately 6 to 25 bar.
  • the expander 82 is the primary drive component for the compressor 80, with the remainder of the driving force being supplied by the turbine 58.
  • the expander 82 obtains its energy from the reaction off-gas supplied through gas line 92 after the off-gas has passed through each of the condensers 20, 22, and 24.
  • the off-gas passes through the condensers 20, 22, and 24, much of the organic materials within the off-gas condense, and that condensate can be returned to the oxidation reactor 14 after various processing.
  • the remaining off-gas can be relatively cold, but is still at relatively high pressure.
  • that off- gas has a temperature of approximately 40 0 C and a pressure of approximately 12 bar. Accordingly, the off-gas comprises substantial energy that can be put to use. While the off-gas could be sent directly to the expander 82, it is typical to first remove corrosive and/or combustible byproduct materials from the off-gas.
  • a catalytic combustion unit (CCU) 100 is used to catalytically oxidize the off-gas into environmentally-compatible materials.
  • CCU catalytic combustion unit
  • An example of such a CCU is described in U.S. Pat. No. 5,961 ,942, which is hereby incorporated by reference.
  • Such a unit 100 can reduce or eliminate through oxidation, any residual oxidation reaction solvent present in the off-gas, and can oxidize byproducts, such as methyl bromide.
  • the off- gas Prior to entering the CCU 100, the off- gas is heated using heat exchangers 96 and 98 to facilitate the oxidation reaction within the CCU.
  • heat exchanger 96 uses high pressure steam from the plant boiler to raise the temperature to approximately 200 0 C to 300°C.
  • the off-gas then passes through the heat exchanger 98 and a gas line 99, and into the CCU 100 for oxidation.
  • Fuel can be supplied to the CCU 100 via a fuel line 102 to assist in the reaction.
  • the reaction within the CCU 100 produces further heat that can be transferred to the heat exchanger 98 by delivering the off-gas, now at a temperature of approximately 400 0 C to 510 0 C, through a further gas line 101 and back into the heat exchanger 98. That heat can then be transferred to the off-gas flowing toward the CCU 100.
  • the off-gas After passing through the CCU 100 and the heat exchanger 98, the off-gas has, for example, a temperature of approximately 300°C to 400 0 C and a pressure of approximately 6 to 14 bar.
  • the gas is then delivered to the expander 82 along a gas line 104 and is used to drive the expander 82, which in turn drives the compressor 80.
  • the off-gas exits the expander 82 at or near atmospheric pressure and flows along gas line 106 to a scrubber 108, which removes any acidic and/or inorganic materials, such as bromine and hydrogen bromide, and then exhausts the gas into the atmosphere via gas line 110.
  • blow-off line 112 and control valve 114 that are connected to the air line 90, and a bypass line 116 and control valve 118 that extend between the air line 90 and the gas line 92.
  • a blow-off line 112 and control valve 114 that are connected to the air line 90
  • a bypass line 116 and control valve 118 that extend between the air line 90 and the gas line 92.
  • the oxidation reactor of an aromatic carboxylic acid production plant must be taken offline.
  • One such circumstance is when the reactor is simply taken offline for cleaning or routine maintenance.
  • a condition arises that requires a reactor shut down.
  • Such conditions are referred to as reactor transient conditions, or just transients. When a transient occurs, the reactor is shut down or "tripped" to avoid damage to equipment and/or harm to those that operate that equipment.
  • a small package boiler e.g., having an approximate 70 te/hr capacity
  • a small package boiler e.g., having an approximate 70 te/hr capacity
  • control valve 76 associated with steam line 78 and the control valve 56 associated with steam line 54 are both opened to enable the flow of high pressure steam from a steam source, such as a plant boiler, to the turbine 58.
  • a steam source such as a plant boiler
  • the steam is at a temperature of approximately 300°C and a pressure of approximately 80 bar and is let down to low pressure steam via control valve 76. That steam drives the turbine 58 to at least partially account for the loss of the steam provided from the condensers 20, 22 and 24 during normal system operation.
  • control valve 118 of bypass line 116 is opened to divert the flow of compressed air from the oxidation reactor 14 to the expander 82, which normally operates using the reactor off-gas.
  • the expander 82 By providing that air to the expander 82, the expander continues to be driven, albeit at a slower speed, and further is maintained at a relatively high temperature so that normal operation of the system 10 can be resumed relatively quickly.
  • the expander 82 can be operated at approximately 300 0 C during the reactor transient, which is only approximately 70 0 C cooler than during normal system operation.
  • the blow- off valve 114 can also be opened, at least partially, so that a portion of the compressed air is vented to the atmosphere.
  • the machine train can be safely operated at approximately 70% to 95% its normal operating speed.
  • the steam and air flows are controlled by a central computer system (not shown) that controls the timing of actuation of all the implicated control valves, as well as the extent to which each open valve is opened.
  • Table I provides an indication of the advantageous results that the above- described control scheme can produce.
  • Three systems are identified in the table, including an existing high-temperature expander system, an existing low-temperature expander system, and a high-temperature expander system in accordance with the present disclosure.
  • the existing high-temperature expander system it is assumed that the expander is operated at approximately 450 0 C under normal operating conditions.
  • the existing low-temperature expander system it is assumed that the expander is operated at approximately 190 0 C under normal operating conditions.
  • the expander is assumed to operate at approximately 370 0 C, as described above.
  • Supplemental steam requirements for each of the start-up case, normal operating case, and reactor trip case are identified as to each system.
  • the electricity loss is identified for each reactor trip case.
  • the machine train can be controllably operated at a significantly reduced speed during reactor transients, which saves costs in terms of reduced supplemental steam and/or supplemental electricity requirements.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention porte sur un système ayant un réacteur d'oxydation conçu pour oxyder une charge d'alimentation aromatique pour produire un acide carboxylique aromatique ; et une série de machines qui fournit de l'air comprimé au réacteur, la série de machines comprenant un compresseur d'air à arbre unique.
PCT/GB2009/002804 2008-12-02 2009-12-02 Systèmes et procédés pour la gestion de régimes transitoires d'un réacteur WO2010064006A1 (fr)

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Application Number Priority Date Filing Date Title
CN200980148568.5A CN102239000B (zh) 2008-12-02 2009-12-02 控制反应器瞬态的系统和方法

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US11923308P 2008-12-02 2008-12-02
US61/119,233 2008-12-02

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0962442A1 (fr) * 1998-06-05 1999-12-08 Mitsui Chemicals, Inc. Procédé de préparation d'acides carboxyliques aromatiques
JP2005213223A (ja) * 2004-01-30 2005-08-11 Mitsubishi Chemicals Corp 芳香族カルボン酸の製造方法
US20050256335A1 (en) * 2004-05-12 2005-11-17 Ovidiu Marin Providing gases to aromatic carboxylic acid manufacturing processes
WO2006102137A1 (fr) * 2005-03-21 2006-09-28 Bp Corporation North America Inc. Recuperation amelioree de l'energie lors de la production d'acides carboxyliques aromatiques
US20070276155A1 (en) * 2006-05-24 2007-11-29 Timothy Alan Upshaw Process for energy recovery and water removal in the preparation of aromatic carboxylic acids
WO2008105085A1 (fr) * 2007-02-28 2008-09-04 Hitachi Plant Technologies, Ltd. Procédé de traitement des gaz de combustion produits par la réaction d'oxydation et de récupération d'énergie

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1696097A (zh) * 2004-05-12 2005-11-16 液体空气乔治洛德方法利用和研究的具有监督和管理委员会的有限公司 向芳族羧酸制备工艺提供气体

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0962442A1 (fr) * 1998-06-05 1999-12-08 Mitsui Chemicals, Inc. Procédé de préparation d'acides carboxyliques aromatiques
JP2005213223A (ja) * 2004-01-30 2005-08-11 Mitsubishi Chemicals Corp 芳香族カルボン酸の製造方法
US20050256335A1 (en) * 2004-05-12 2005-11-17 Ovidiu Marin Providing gases to aromatic carboxylic acid manufacturing processes
WO2006102137A1 (fr) * 2005-03-21 2006-09-28 Bp Corporation North America Inc. Recuperation amelioree de l'energie lors de la production d'acides carboxyliques aromatiques
US20070276155A1 (en) * 2006-05-24 2007-11-29 Timothy Alan Upshaw Process for energy recovery and water removal in the preparation of aromatic carboxylic acids
WO2008105085A1 (fr) * 2007-02-28 2008-09-04 Hitachi Plant Technologies, Ltd. Procédé de traitement des gaz de combustion produits par la réaction d'oxydation et de récupération d'énergie

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