WO2014179043A1 - Dispositif d'autoclave chemisé pour la production de polyamides - Google Patents

Dispositif d'autoclave chemisé pour la production de polyamides Download PDF

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Publication number
WO2014179043A1
WO2014179043A1 PCT/US2014/034145 US2014034145W WO2014179043A1 WO 2014179043 A1 WO2014179043 A1 WO 2014179043A1 US 2014034145 W US2014034145 W US 2014034145W WO 2014179043 A1 WO2014179043 A1 WO 2014179043A1
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Prior art keywords
autoclave
heating
polymerization
vessel body
heating conduit
Prior art date
Application number
PCT/US2014/034145
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English (en)
Inventor
Leen Monster
Leonardus J. MOLENDIJK
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INVISTA North America S.à r.l.
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Publication date
Application filed by INVISTA North America S.à r.l. filed Critical INVISTA North America S.à r.l.
Priority to EP14724603.7A priority Critical patent/EP2991757A1/fr
Publication of WO2014179043A1 publication Critical patent/WO2014179043A1/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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • 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
    • B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • 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
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00081—Tubes
    • 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
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/0009—Coils
    • 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
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • B01J2219/0236—Metal based
    • 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
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
    • B01J2219/0277—Metal based
    • B01J2219/0286—Steel

Definitions

  • the present disclosure is drawn to polymerization autoclaves which utilize exterior heating coil alloys that substantially avoid low cycle fatigue damage from repeated cyclic temperature differentials.
  • Continuous and batch polymerization processes are utilized for a variety of polymer production facilities. Each process has advantages and drawbacks depending on a variety of variables such as capital costs, throughput, polymer type, polymerization kinetics, and other priorities.
  • Batch polymerization processes typically utilize a polymerization reactor or autoclave which is heated to an appropriate process temperature. Polymerization autoclaves can most often be designed to tolerate high temperatures and pressures during processing.
  • Heating of such polymerization reactors typically involves the use of closed loop heating systems which transfer heat from a heating fluid into the reactor.
  • Heating systems can include exterior heating coils, internal heating loops, jacketed systems, or other similar heat transfer systems.
  • Such systems can have inherent limitations in terms of heat distribution, heating rates, reliability, and operational constraints. As such, improvements to such heating systems on polymerization reactors continue to be sought and developed.
  • a polymerization autoclave having an exterior heating assembly can include an autoclave vessel body, an autoclave inlet, a pressure release valve, and a heating conduit.
  • the autoclave vessel body defines an interior reaction chamber within which a polymerization reaction can occur.
  • the vessel body has an outer surface and an inner surface having a vessel wall thickness.
  • the vessel body is also formed of a steel alloy.
  • the autoclave inlet is oriented through the autoclave vessel body and is capable of directing polymerization reactants into the interior reaction chamber.
  • the pressure release valve is in fluid
  • the heating conduit is wrapped around and attached to a heat transfer portion of the outer surface.
  • the heating conduit has multiple wraps around the autoclave vessel body such that heating fluid can be circulated through the heating conduit to transfer heat into the interior reaction chamber across the heat transfer portion.
  • the heating conduit also has a heating conduit wall thickness and is formed of a chromium-molybdenum steel alloy.
  • the heating conduit is also attached to the heat transfer portion so as to substantially avoid low cycle fatigue damage from repeated cyclic temperature differentials greater than 80 °C.
  • a method of assembling a polymerization autoclave having an exterior heating assembly can comprise providing an autoclave vessel body, wrapping a heating conduit around the heat transfer portion of the out surface multiple times, and welding the heating conduit to the heat transfer portion.
  • the autoclave vessel can define an interior reaction chamber and can have an outer surface with a heat transfer portion and an inner surface for containing reactants.
  • the autoclave vessel body can also be formed of a steel alloy and having a vessel wall thickness.
  • the assembly can be such that the heating fluid can be circulated through the heating conduit to transfer heat across the heat transfer portion into the interior reaction chamber.
  • the heating conduit can have a heating conduit wall thickness and can be formed of a chromium-molybdenum steel alloy so as to substantially avoid low cycle fatigue damage from repeated cyclic temperature differentials greater than 80 °C.
  • FIG. 1 is a cross-sectional view of a polymerization autoclave in
  • compositions comprising, “comprising,” “containing” and “having” and the like can have the meaning ascribed to them in U.S. Patent law and can mean “includes,” “including,” and the like, and are generally interpreted to be open ended terms.
  • the term “consisting of” is a closed term, and includes only the devices, systems, methods, components, structures, steps, or the like specifically listed, and that which is in accordance with U.S. Patent law.
  • Consisting essentially of or “consists essentially” or the like when applied to devices, systems, methods, components, structures, steps, or the like encompassed by the present disclosure refers to compositions like those disclosed herein, but which may contain additional structural groups, composition components, or method steps, etc.
  • compositions or methods do not materially affect the basic and novel characteristic(s) of the compositions or methods, compared to those of the corresponding compositions or methods disclosed herein.
  • phrases such as “suitable to provide,” “sufficient to cause,” or “sufficient to yield,” or the like, in the context of methods of synthesis refers to reaction conditions related to time, temperature, solvent, reactant concentrations, and the like, that are within ordinary skill for an experimenter to vary to provide a useful quantity or yield of a reaction product. It is not necessary that the desired reaction product be the only reaction product or that the starting materials be entirely consumed, provided the desired reaction product can be isolated or otherwise further used.
  • ratios, concentrations, amounts, and other numerical data may be expressed herein in a range format. It is to be understood that such a range format is used for convenience and brevity, and thus, should be interpreted in a flexible manner to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range includes "about 'x' to about 'y'".
  • a concentration range of "about 0.1 % to about 5%” should be interpreted to include not only the explicitly recited concentration of about 0.1 wt% to about 5 wt%, but also include individual concentrations (e.g., 1 %, 2%, 3%, and 4%) and the sub-ranges (e.g., 0.5%, 1.1 %, 2.2%, 3.3%, and 4.4%) within the indicated range.
  • the term “about” can include traditional rounding according to significant figures of the numerical value.
  • the phrase “about 'x' to 'y” includes “about 'x' to about 'y'”.
  • embodiments of the present disclosure employ, unless otherwise indicated, techniques of chemistry, metallurgy, welding, and the like, which are within the skill of the art.
  • the materials are extruded or otherwise removed from the autoclave.
  • Such processes introduce significant cyclic variations in temperatures within the autoclave, along the autoclave walls, and along adjacent heating systems such as external heating coils.
  • differentials in temperatures across each portion of the autoclave and heating system can create mechanical stresses at weld joints and adjacent materials.
  • formation of dyadic polyamides such as nylon 6,6 can involve converting/reacting nylon salt to form nylon polymer at elevated temperatures around 189-250 °C for several hours.
  • Autoclave wall temperatures are initially below typical heating fluid temperatures.
  • Temperature and pressure conditions in a nylon 6,6 batch process cycle include variations during initial startup, charging of nylon salt, reaction stages, extrusion stage, and clean out stages. Among these various stages, temperatures changes create temperature differentials between the autoclave walls and heating coils.
  • Table 1 provides one example of cyclic polymerization operating conditions.
  • the temperature differential between the heating coil and the autoclave wall can vary dramatically. External heating coils are most often welded to outer surfaces of the autoclave. During start-up of the reactor, expansion of the heating coil is restrained by the relatively cooler autoclave walls. This results in a compression load which may exceed elastic deformation limits of the welds. Such permanent deformation leads to stress in weld joints as autoclave walls subsequently heat up to normal operating temperatures. Similar deformation results during variations in temperature conditions such as boil out, steam cleaning, washing, shutdown and startup of the reactor. In each case, changes in temperature results in a variable temperature gradient across the weld as a function of time. Furthermore, as a vessel is used over and over again for multiple batch cycles during normal use, temperatures are cycled from low to high within the various batch cycles.
  • a polymerization autoclave 100 can include an autoclave vessel body 104 and an exterior heating assembly 102 which includes a heating conduit 1 10. Also included is a plurality of ports at a top end of the vessel for transferring reactant and/or additives into the vessel, venting gases, etc. Any of these inlet/outlet ports (or others that can be optionally included) can be used for these purposes.
  • the vessel might be designed to have an autoclave inlet 106, a pressure release valve 108, and an optional secondary inlet, though other arrangements can be used as may be practical for a given polymerization process.
  • the autoclave vessel body defines an interior reaction chamber 1 12 within which a polymerization reaction can occur.
  • the polymerization reaction can be adapted for the formation of polyamides such as nylon 6,6, although other polymerization reactions can also be suitable.
  • the autoclave vessel body 104 can be any vessel in which a
  • suitable vessel bodies can include an interior reaction chamber which is enclosed by an autoclave wall and capable of pressurization. Although operating conditions can vary, the autoclave vessel body can be adapted to retain pressures of at least 300 psia, and in some cases at least 600 psia.
  • the autoclave vessel body can have an outer surface 1 14 and an inner surface 1 16.
  • the autoclave vessel body has a cylindrical central portion 1 18, with a domed top portion 120, and a conical bottom portion 122. Other shapes can likewise be used.
  • the autoclave vessel body can be formed as a single unitary vessel. Alternatively, the autoclave vessel body can be formed of multiple segments.
  • Such segmentation of the autoclave vessel body can facilitate manufacture, assembly, cleaning, and repair of the device.
  • an internal heating assembly 124 can be engaged through the conical bottom portion of autoclave vessel body.
  • the polymerization autoclave can be assembled and disassembled by removing fasteners along flange 126 to allow removal of the internal heating assembly as a single unit. Additional features can be provided as part of the polymerization autoclave for convenience and improved performance.
  • retainer 127 can be connected to a fixed structural member to provide mechanical stability to the autoclave.
  • the autoclave vessel body can be formed of materials which are structurally sufficient to withstand expected operating conditions.
  • the autoclave vessel body is typically formed of a steel alloy.
  • suitable steel alloys can include carbon steel alloys (e.g. HII carbon steel, St35.8, P235GH, P265GH, P295GH, P355GH, or the like), refractory metal alloys, composites thereof, and combinations thereof.
  • the vessel walls can be formed of a chromium- molybdenum steel alloy.
  • Suitable chromium-molybdenum steel alloys can include, but are not limited to, 16Mo3, 13CrMo4-5, P235GH, P265GH, and combinations thereof.
  • the vessel walls can be formed of 16Mo3 which exhibits desirable properties over a wide range of operating conditions.
  • Table 2 outlines chemical compositions for these chromium- molybdenum steel alloys. Table 2: Chromium-Molybdenum Steel Alloys (balance Fe)
  • the autoclave vessel body can be a cladded vessel having a primary vessel wall and at least one interior cladding layer coated on the inner surface.
  • Such cladding layers can provide increased resistance to corrosion beyond materials used for the primary vessel wall.
  • the cladded walls can often represent a compromise to achieve both mechanical integrity which is characteristic of the primary vessel wall and corrosion resistance which is characteristic of the cladding layers.
  • the primary vessel wall can be coated on interior surfaces with at least one interior cladding layer.
  • Cladding can be coated on the primary vessel wall using known techniques such as explosion welding, although other deposition techniques may be suitable. Cladding layer materials can also provide corrosion protection to inner surfaces which are in contact with polymerization reactants and products at high temperatures and pressures.
  • the primary vessel wall can be formed of steel alloys as outlined above, and in one optional aspect are formed of a carbon steel alloy such as HII carbon steel or St35.8.
  • the primary vessel wall can be formed of a chromium-molybdenum steel alloy such as those described above.
  • the interior coating layer can be stainless steel (e.g. SS321 , 314 and 306), or the like.
  • stainless steel 321 alloys can include X6CrNiTi18-10, X12CrNiTi8-9, or the like. Table 3 outlines nominal chemical compositions for several suitable stainless steels. Table 3: Stainless Steel Chemical Composition
  • Thicknesses of the autoclave vessel body 104 can vary. Vessel thickness can substantially affect rates of heat transfer during temperature transitions and can also vary degree of thermal expansion and contraction during such temperature transitions as well. Accordingly, vessel wall thicknesses can vary but are generally from about 15 mm to about 50 mm, and in many cases from about 20 mm to 40 mm. In the case of cladded vessels, the primary vessel wall can often have a thickness from 20 mm to 28 mm and the cladding layer can include a single cladding layer having a thickness of 1 .5 mm to 5 mm. In one example, the vessel wall thickness can be 24 mm carbon steel (HII) with a 3 mm stainless steel 321 interior cladding.
  • HAI 24 mm carbon steel
  • the conical bottom portion 122 can have a wall thickness which is larger than a wall thickness of the cylindrical central portion 1 18.
  • the conical bottom portion thickness can be about 10% to 40% greater than the cylindrical central portion wall thickness.
  • Various ports, inlets, and outlets can be formed in the autoclave vessel body 104. Such features can provide for control of feedstock, product removal, pressure control, venting, introduction of additives, introduction of staged polymerization reactants, temperature probes, pressure probes, cleaning, video feed, and the like.
  • inlets can be configured for any of these purposes, the autoclave inlet 106 is oriented through the autoclave vessel body and is capable of directing polymerization reactants into the interior reaction chamber 1 12.
  • the autoclave inlet can be sufficiently wide to allow for introduction of reactants quickly to reduce charging time.
  • any suitable inlet diameter can be used, the autoclave inlet often has a diameter from 1 inch to 4 inches, and in many cases about 3 inches.
  • the pressure release valve 108 can be in fluid communication with the interior reaction chamber 1 12. More specifically, the pressure release valve is also capable of selectively discharging vapor from the vapor space of the interior reaction chamber and is most often oriented within the domed top portion 120 of the autoclave vessel body 104.
  • the pressure release valve is illustrated as a flanged conduit; however any suitable pressure release valve can be operatively connected to the flange.
  • the pressure release valve can often be adjustable in order to provide for variable pressure within the interior reaction chamber throughout each polymerization process cycle. Such adjustable pressure relief valves can be operatively connected to a process controller module for remote control of pressure conditions, along with other monitored and controlled conditions.
  • the secondary inlet 128 can be oriented in the domed top portion.
  • This secondary inlet can be used for addition of additives during processing, staged polymerization reactants or other components.
  • additives can include colorants, ultraviolet stabilizers, plasticizers, cross-linking agents, anti-microbials, fillers, process aids, flame retardants, biodegradability enhancers, and the like.
  • Optional spray nozzles can be oriented on internal ends of inlets described herein.
  • inlets which introduce material into the interior reaction chamber 1 12 can terminate a distance away from the interior wall surface 1 16. Accordingly, in order to more uniformly distribute such materials into the interior reaction chamber, nozzles can be used to increase and control dispersion patterns.
  • Polymerization processing can often involve careful control of reaction temperatures within the interior reaction chamber 1 12. Such control of
  • the exterior heating assembly 102 can include a heating conduit 1 10 which is wrapped around the autoclave vessel body 104.
  • the outer surface 1 14 can include an exposed portion and a heat transfer portion.
  • the heating conduit can be directly attached to the heat transfer portion of the outer surface.
  • the exposed portion of the outer surface is free of heating mechanisms and is exposed to surrounding environment.
  • the heating conduit has multiple wraps around the autoclave vessel body such that heating fluid can be circulated through the heating conduit to transfer heat into the interior reaction chamber across the heat transfer portion.
  • the number of wraps can vary considerably, but is often more than ten wraps, and in some cases up to or more than twenty.
  • the exterior heating assembly can cover the heat transfer portion of the outer surface. Although degree of coverage can vary, the exterior heating assembly can cover from 30% to 80% of the outer surface, in some cases 5% to 70%, and often from 40% to 70% of the outer surface. With respect to surface coverage, gaps between windings in the heating conduit are included in these percentages as covered by the exterior heating assembly.
  • Each wrap typically has a small gap such that the outer surface 1 14 is exposed in between successive wraps of the heating conduit 1 10.
  • gaps are generally limited in order to improve heat transfer into the autoclave, but are most often limited to no more than 50% (and in many cases less than 20%) of the width of surrounding heating conduit.
  • the heating conduit can also be formed having a variety of cross-sectional shapes such as, but not limited to, half-pipe, full-pipe, U-channel, V-channel, and the like.
  • the heating conduit can have a half-pipe cross-sectional shape.
  • the heating conduit can have an overlapping cross-section where one edge is welded to the outer surface of the autoclave vessel body, while an opposing edge is welded to a suspended portion (i.e.
  • the heating conduit can typically have a uniform cross-sectional shape along an entire length of the heating conduit which is attached to the outer surface.
  • conduit wall thickness can be varied and is generally less than the vessel wall thickness.
  • Corresponding wall thicknesses of the heating conduit can also affect the degree of stress transferred to the heating coils during transitions in temperatures. Heating conduit wall thicknesses are generally less than about 25 mm. In one example, the heating conduit wall thickness can be from about 3 mm to about 6 mm and in a specific example 4 mm.
  • a ratio of vessel wall thickness to the conduit wall thickness can influence performance. As a general guideline, the ratio of vessel wall thickness to conduit wall thickness can be 2: 1 to 15:1 , and in some cases 5:1 to 9:1 .
  • Heating conduit thickness can affect stress induced in welds, as well as heat losses to surrounding environment.
  • outer width of the heating conduit 1 10 can also determine percentage coverage of the outer surface 1 14 for purposes of heat transfer.
  • cross-sectional heating conduit profiles can also determine patterns of heat flow within the conduit.
  • heating conduit height i.e. perpendicular distance from the outer surface to a distal portion of the heating conduit
  • excessive heights can result in undesirable heat currents and increased heating fluid volume requirements.
  • increased outer width i.e. width of heating fluid contact area with the outer surface
  • a reduction in the number of contact points with the outer surface results in fewer welds and potential failure points.
  • excessively wide conduits can also result in non-uniform heat flow patterns.
  • the outer width of heating conduits can vary considerably, such as from about 50 mm to about 100 mm.
  • the heating conduit 1 10 can be formed in whole or in part as a jacketed chamber which circumvents at least a portion of the heat transfer portion of the outer surface 1 14 of the autoclave vessel body 104.
  • a jacketed chamber can optionally include internal baffles or walls which direct the heating fluid across portions of the outer surface.
  • baffle arrangements can be used, although complex and or numerous baffle configurations can cause excessive pressure head. Such increased pressure within the heating assembly can increase chances of causing a failure within the heating assembly, need for high pressure heating fluid pumps, or increased operational costs.
  • the heating conduit 1 10 can be formed of a material which is operable at temperatures of at least 350 °C with repeated heating and cooling cycles.
  • heating conduits which are formed of a chromium- molybdenum steel alloy.
  • suitable chromium- molybdenum steel alloys include 16Mo3, 13CrMo4-5, P235GH, P265GH, and combinations thereof. Chemical compositions of these chromium-molybdenum steel alloys are provided in Table 4.
  • the heating conduits 1 1 0 can be formed of a dissimilar steel alloy from the autoclave vessel body 104 and in particular the outer surface 1 14.
  • the heating conduits can be formed of the same steel alloy as used in formation of the autoclave vessel body, especially the outer surface.
  • the exterior heating assembly 102 can be welded to the outer surface 1 14 of the autoclave vessel body 104 using a high temperature weld alloy.
  • suitable weld alloys can include, Mn-Mo alloys, W2 Mo, G 46 AM G4MO, E Mo B32 H5, AG42, W 42 5 W2Si, or combinations thereof.
  • the weld alloy can be AG42.
  • the weld alloy can be W2 Mo.
  • Commercial weld alloys which can be suitable include filler metals such as, but not limited to, Nertalic 86®, Union® l-Mo, or SL® 12G.
  • the exterior heating assembly 102 can include an external heating inlet 130 where heating fluid is introduced.
  • the heating conduit can thus have an exterior heating outlet 132 which allows the heating fluid to be recirculated and reheated.
  • the exterior heating assembly 102 can be welded to the outer surface 1 14 using any number of welding techniques.
  • welding techniques include gas tungsten arc welding (GTAW), shielded metal arc welding (SMAW), gas metal arc welding (GMAW), and the like.
  • GTAW gas tungsten arc welding
  • SMAW shielded metal arc welding
  • GMAW gas metal arc welding
  • Overlapping offset weld deposits in building up weld joints can be used to increase weld joint strength.
  • weld joints can be full penetration welds (i.e. as opposed to tack welds or partial penetration welds).
  • root spacing of weld joints can be 1 mm to 5 mm, although other spacing may be suitable.
  • the heating conduit can be attached to the heat transfer portion of the outer surface 1 14 so as to
  • heating fluids substantially avoid low cycle fatigue damage from repeated cyclic temperature differentials greater than 80 °C, and in some cases greater than 100 °C.
  • heating fluids include Thermanol 66® (a proprietary mixture of hydrogenated terphenyl, partially hydrogenated quaterphenyls and higher polyphenyls, and terphenyl), Dowtherm® (mixture of biphenyl and diphenyl oxide), and mixtures thereof.
  • Suitable heating fluids can operate at temperatures from 330 °C to 340 °C and have a vapor pressure less than 100 psi.
  • the polymerization autoclave 100 can include the interior heating assembly 124 which includes internal heating manifolds.
  • an internal heating manifold can include a conical reservoir 134 having an inlet 136.
  • the conical reservoir can be housed within the conical bottom portion 122 of the autoclave which is attached to the vessel body at flange 126.
  • the internal heating manifold can further include one or more heating tubes 138 which are each fluidly connected to the conical reservoir.
  • the heating tubes can be connected to a common outlet 140 for recycling and/or reheating of cooled heating fluid.
  • the heating tubes can be vertically oriented and substantially parallel to one another.
  • heating tubes can be oriented within a lower region of the interior reaction chamber 1 12 to form an axially oriented annular heating manifold.
  • An optional upper housing 142 can be provided to distributed heat more uniformly within the interior reaction chamber.
  • the upper housing illustrated has a ring shape and a square cross-section with a peaked ceiling.
  • the internal heating tubes can be formed of any material which is operable up to at least 350 °C and in some cases up to about 400 °C.
  • suitable materials can include those previously listed for use with the autoclave vessel walls, exterior heating conduit, stainless steel, and the like.
  • the internal heating tubes can be formed of a stainless steel.
  • stainless steels include stainless steel 304, 316 and 321 .
  • the interior heating assembly 124 can be integrally connected to a portion of the conical bottom 122 which can be removed as a single unit. Such segmentation of the autoclave vessel body can facilitate manufacture, assembly, cleaning, and repair of the device. Furthermore, the conical bottom portion 122 includes an autoclave outlet 144 which allows for removal of product from the interior reaction chamber 1 12 for further processing (e.g. extrusion, drawing into fiber, molding, etc.)- Extrusion can be performed by increasing pressure within the interior reaction chamber 1 12 and optionally increasing temperatures in order to decrease viscosity of polymerization products.
  • the polymerization autoclave 100 can be an agitated autoclave which includes an internal mixer (not shown).
  • the internal mixer can typically be oriented vertically along a centerline of the interior reaction chamber 1 12. Internal mixers can allow for increased uniformity of polymerization conditions and decreases in polymerization reaction times. In such cases, the internal heating assembly 124 can be omitted or reconfigured to provide clearance for operation of the internal mixer.
  • polymerization autoclaves and configurations described herein can provide effective heat transfer, while also minimizing or eliminating chances of low cycle fatigue.
  • polymerization autoclaves incorporating such features can provide increased service life, higher reliability, and more uniform heat distribution.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente invention concerne un autoclave de polymérisation ayant un ensemble de chauffage extérieur qui peut comprendre un corps de cuve d'autoclave, une entrée d'autoclave, une soupape de surpression, et un conduit de chauffage. Le corps de cuve d'autoclave délimite une chambre de réaction intérieure dans laquelle peut se produire une réaction de polymérisation. Le corps de cuve d'autoclave est également en alliage d'acier. Le conduit de chauffage enveloppe une partie de transfert de chaleur de la surface externe et y est fixé. Le conduit de chauffage présente de multiples enveloppes autour du corps de cuve d'autoclave de sorte que le fluide de chauffage puisse circuler dans le conduit de chauffage afin de transférer la chaleur dans la chambre de réaction intérieure à travers la partie de transfert de chaleur. Le conduit de chaleur est formé d'un alliage d'acier chrome-molybdène. Le conduit de chauffage est également fixé à la partie de transfert de chaleur de manière à empêcher essentiellement un dommage résultant de la fatigue oligocyclique provenant de différences de température cycliques répétées supérieures à 80 °C.
PCT/US2014/034145 2013-05-01 2014-04-15 Dispositif d'autoclave chemisé pour la production de polyamides WO2014179043A1 (fr)

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EP14724603.7A EP2991757A1 (fr) 2013-05-01 2014-04-15 Dispositif d'autoclave chemisé pour la production de polyamides

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US201361817987P 2013-05-01 2013-05-01
US61/817,987 2013-05-01

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CN (2) CN113648931A (fr)
TW (1) TW201505708A (fr)
WO (1) WO2014179043A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
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CN117065660A (zh) * 2023-10-13 2023-11-17 常鑫防水科技股份有限公司 一种彩色水性聚氨酯防水涂料热反应设备及其控制方法

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US3759879A (en) * 1971-05-28 1973-09-18 Firestone Tire & Rubber Co Continuous bulk polymerization process for vinyl chloride copolymers
US3909207A (en) * 1973-03-09 1975-09-30 Monsanto Co Vertical stirred mass polymerization apparatus
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CN105056863B (zh) * 2015-07-29 2017-08-08 江苏建亚环保科技股份有限公司 带有刮料装置的树脂生产用反应釜
CN117065660A (zh) * 2023-10-13 2023-11-17 常鑫防水科技股份有限公司 一种彩色水性聚氨酯防水涂料热反应设备及其控制方法
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