WO2017178323A1 - Réacteur de polymérisation à petite échelle - Google Patents

Réacteur de polymérisation à petite échelle Download PDF

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Publication number
WO2017178323A1
WO2017178323A1 PCT/EP2017/058218 EP2017058218W WO2017178323A1 WO 2017178323 A1 WO2017178323 A1 WO 2017178323A1 EP 2017058218 W EP2017058218 W EP 2017058218W WO 2017178323 A1 WO2017178323 A1 WO 2017178323A1
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WO
WIPO (PCT)
Prior art keywords
reactor
stirrer
reactor vessel
blades
baffle
Prior art date
Application number
PCT/EP2017/058218
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English (en)
Inventor
Tom SCHOFFELEN
Frans VISSCHER
Francesco Bertola
Nicolaas Hendrika Friederichs
Original Assignee
Sabic Global Technologies B.V.
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Filing date
Publication date
Application filed by Sabic Global Technologies B.V. filed Critical Sabic Global Technologies B.V.
Publication of WO2017178323A1 publication Critical patent/WO2017178323A1/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
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00831—Stationary elements
    • B01J2208/0084—Stationary elements inside the bed, e.g. baffles
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00858—Moving elements
    • B01J2208/00867—Moving elements inside the bed, e.g. rotary mixer
    • 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
    • B01J2219/00011—Laboratory-scale plants
    • 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
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/00768—Baffles attached to the reactor wall vertical
    • 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
    • B01J2219/19—Details relating to the geometry of the reactor
    • B01J2219/194—Details relating to the geometry of the reactor round
    • B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
    • B01J2219/1943—Details relating to the geometry of the reactor round circular or disk-shaped cylindrical

Definitions

  • the invention relates to a small scale polymerization reactor for the preparation of polymers and a method of preparing polymers using the reactor,.
  • Such process development reactors have reactor vessels, usually in a range of 1 liter in volume or less.
  • Translatability from small scale tot medium and/or large scale is a challenge, since process conditions differ between small scale and medium or large scale, Especially when these small scale reactors involve the chemical transformation of gaseous chemicals into suspended or dissolved polymers in a diluent, the volumetric gas-liquid mass transfer rates of a gas in a polymer suspension in small scale reactors can be too low.
  • the volumetric gas- liquid mass transfer rate of monomer gas into a viscous solution of an ethylene containing polymer in a hydrocarbon diluent may show considerable difference between small scale processes and medium and/or large scale processes.
  • the exact composition of the gaseous phase as the composition of the gaseous phase translates into a certain composition of the polymer.
  • the molecular mass of the resulting polyolefin can be regulated by the addition of hydrogen.
  • the ratio of hydrogen to ethylene in the gaseous phase the molar mass of the resulting polymer can be steered.
  • the incorporation of 1-butene in the resulting polymer can be adjusted by changing the ratio of 1-butene to ethylene in the gaseous phase.
  • the sampling lines are of low volume, which is reached by having a small inner diameter of the sampling lines. This creates a challenge, as one has to prevent that liquid or solid components can enter into the sampling line and as a result would block the feed to the analytical device.
  • the distance between the liquid level and the sampling line is relatively large because of the large scale of the reactor.
  • the distance is intrinsically short due to the dimensions of such small reactors. Therefore one has to prevent that liquids or solids splash onto the upper part of the reactor and could subsequently block the feeding lines to the analytical device. Usage of a filter at the entrance of the feeding line to the analyzer often only postpones the blockage of the lines to the analyzer.
  • the volumetric gas-liquid mass transfer rate of ethylene gas into a hydrocarbon diluent is a challenging task. For instance, it is desirable that the rate of the catalytic conversion of dissolved ethylene into polyethylene, which takes place in the diluent, does not exceed the volumetric gas-liquid mass transfer rate of ethylene from the gas into the diluent. Only when the volumetric gas-liquid mass transfer rate of ethylene into the diluent is higher than the catalytic conversion, one can fully benefit from the intrinsic performance of the catalyst, like for example productivity.
  • a value for volumetric gas-liquid mass transfer coefficient of 0,023 per second may be obtained, and a value of 0.030 can be targeted to avoid entering into starved conditions (Gas-Liquid Mass Transfer Coefficient in Stirred Tank Reactors - Archis A. Yawalkarl , Albertus B.M. Heesink2, Geert F. Versteeg2 and Vishwas G. Pangarkarl ).
  • Translatability from small scale reactors to large scale reactors is low in this field.
  • the volumetric gas-liquid mass transfer rate of materials used in the processing can be improved by various measures such as increasing stirring efficiency, reactor configuration and pressure. Each measure has its own limitation.
  • Stirrer efficiency can be improved by for example high stirrer rotation speed and stirrer type, i.e. blades configuration, number of blades.
  • stirrer rotation speeds cannot be increased unlimited and the choice in stirrer types is limited.
  • baffle In medium or large scale reactors, a baffle can be used for mixing improvement.
  • a baffle In small scale polymerization reactors is uncommon. Baffles limit space inside the small reactor vessels and are prone to contamination by deposits inside the reactor vessels. High stirrer speeds however may lead to spattering and splashing of the polymer suspension, which is undesirable as this may cause plugging of the sampling line in overhead reactor vessel covers. Instrumentation within the reactor vessel, such as sensors or fluid inlets for measurements, may cause turbulent flow within the reactor vessel, however such elements generally do not provide a controlled flow profile, sufficient for improving the volumetric gas-iiquid mass transfer rate.
  • feed lines for supplying monomer and other components for performing polymerization under experimental conditions are known, which may extend into a development reactor vessel, however such feed lines are also not known to provide additional disturbances to the polymer suspension and polymer suspension surface, to sufficiently improve the stirring and obtain the desired volumetric gas-liquid mass transfer rate. Moreover it is described that such feed lines have narrow inner diameters. Therefore it is undesirable to extend such feed lines into the polymer suspension, as the polymer particles or catalyst particles may cause plugging of the inner channel of the feed lines. In addition, at high stirrer speeds, there is a high probability of splashing of polymer particles throughout the complete inner part of the reactor, which in turn would cause eventual installed sampling lines to plug.
  • the reactor system from EP1310296 has no integrated analytical device that measures the composition of the headspace of the reactors, making it less suitable to use for accurate product development.
  • International published patent application WO02/081076 shows a combinatorial chemistry reactor system for the parallel processing of reaction mixtures.
  • the system comprises a frame, a head mounted in fixed position on the frame, and a reactor block having a plurality of wells therein for containing reaction mixtures.
  • the reactor block is movable with respect to the head between a first position in which the reactor block and head are assembled for conducting reactions in the wells and a second position in which the reactor block is removed from the head for providing access to the vessels. Gaps in the reactor block between the wells serve to thermally isolate the wells from one another.
  • the reactor has wells in which stirrers are present for stirring a reaction mixture. Also a sensing device is described which can be present in the wells, which may enhance the stirring.
  • the reactor system from WO02/081076 has no integrated analytical device that measures the composition of the headspace of the reactors, making it less suitable to use for accurate product development.
  • instrumentation such as a temperature sensor extending into the polymer suspension does not provide a sufficient volumetric gas-liquid mass transfer rate in processes for ethylene polymerization, wherein solid particles are obtained, sufficient for translatability of the small scale process to medium or large scale processes.
  • Michael Lallemand [2] describes the performances of Ni-exchanged MCM-41 mesoporous materials as catalysts for ethylene oligomerization with a continuously stirred tank reactor (CSTR). It describes the use of a high speed agitator, rotating at speeds of 1000 rpm. A CSTR with agitator at this speed may provide effective oligomerization resulting mainly in C4, C6, C8 and CIO olefins.
  • the reactor according to the invention comprises a reactor vessel for holding a polymer suspension, wherein the reactor has a volume of less than one liter and wherein a reactor vessel height versus a reactor vessel diameter is greater than or equal to two.
  • the reactor further comprises a drive shaft extending into the reactor vessel having attached at least one stirrer, each stirrer has at least three, more preferably four, stirrer blades, and the stirrer blades are positioned in a lower part of the reactor vessel.
  • the drive shaft is driven by a drive causing rotation of the stirrer, the drive is preferably capable of stirring the stirrer at a speed in a range of 1000 rpm or less. More preferably the drive is capable of driving the stirrer at a speed in a range of 800 - 1000 rpm. This keeps the stirring speed sufficiently low to prevent splashing of the polymer suspension.
  • the at least one stirrer is arranged for having an axial flow profile parallel to a central axis of the reactor vessel coinciding with the drive shaft.
  • the at least one stirrer can comprise an axial impeller.
  • the flow profile ensures that the polymer suspension attains an axial motion in the reactor vessel near the drive shaft and another axial motion with in opposite direction near the reactor vessel wall.
  • the flow profile allows high rate dissolution of the monomer into the polymer suspension.
  • the opposite axial polymer suspension flow near the drive shaft and near the reactor vessel wall causes a radial flow of polymer suspension from the center of the reactor vessel towards the reactor vessel wall or vice versa.
  • the stirrer also causes a rotary motion of the polymer suspension in the reactor vessel around a central reactor vessel axis, coinciding with the drive shaft.
  • the limited rotation speed of the stirrer prevents the polymer suspension to splash, thereby preventing the sampling line inlet to be plugged by the polymer suspension.
  • high rate volumetric gas-liquid mass transfer rate can be achieved whilst preventing plugging of the sampling line inlet.
  • the small scale polymerization reactor allows translatabiiity of the small scale process to a medium or large scale process
  • the aspect ratio of the reactor vessel i.e. the reactor vessel height versus reactor vessel diameter is greater than or equal to two.
  • a higher aspect ratio has various advantages, such as better transportability, relatively small foot print, and also reduced wall thickness so less wall material is necessary.
  • a stirrer fitted in a reactor vessel with high aspect ratio needs less power due to its reduced radius, and will exhibit lower mixing intensity variation.
  • the reactor further comprises a reactor vessel cover, for overhead covering the top of the reactor vessel.
  • the reactor vessel cover comprises at least one sampling line inlet accommodated in the cover for monitoring, in use of the reactor, a gas phase composition. In this way, gaseous components of the reaction mixture can be fed from the reactor to an analytical device via the sampling lines.
  • the stirrer has four stirrer blades. This provides optimal volumetric gas- liquid mass transfer rates within the given speed range of less than 1000 rpm, and preferably 800 - 1000 rpm.
  • the reactor furthermore comprises a baffle that is top mounted and the baffle is mounted to a structure extending above the reactor vessel.
  • the at least two baffle blades are mounted to a side of the reactor vessel cover that, in use of the reactor, is arranged to face the interior of the reactor vessel. In this way, the baffle can be extracted from the reactor vessel when reactor vessel and reactor cover are separated. This allows adequate cleaning of the reactor vessel and of the baffle blades, further preventing undesired deposits.
  • the at least two baffle blades In use of the reactor, the at least two baffle blades partially extend along an inner side of an upper part of the reactor vessel with a length in a range of 40% to 70% of the reactor vessel height to a level above the at least one stirrer. This allows a stirrer to be installed underneath the lower side of the baffle blades. Furthermore, each one of the at least two baffle blades, as seen in use of the reactor in a direction perpendicular to a reactor vessel wall next to which it is arranged, has an elongated cross-section and a blade width in a range of 2% to 10% of the reactor vessel diameter.
  • the baffle blades divert the rotational flow and also cause a radial flow of the polymer suspension from the reactor vessel wall towards the center of the reactor vessel towards the drive shaft connected to the stirrer or vice versa.
  • the radial flow at the surface of the polymer suspension can cause an improved monomer volumetric gas-liquid mass transfer rate.
  • baffle blades which partially extend into the reactor vessel prevent deposit of polymer especially in the lower part of the reactor vessel and allow space for the stirrer in the lower part of the reactor vessel In use, the baffle blades extend into the liquid phase of the polymer suspension, at least causing disturbance of the polymer suspension surface, to improve contact between liquid phase and monomer gas phase.
  • At least two baffle blades are spaced evenly along the inner side of the reactor vessel wall. This allows a more homogenous distribution of the polymer suspension within the reactor vessel.
  • the at least one stirrer is configured to' establish, in use of the reactor, a flow profile in the polymer suspension that is radially inward and axially downward. This causes the polymer suspension to be axially drawn down from the top center part of the reactor vessel to be pushed downward and radially outward towards the reactor vessel, to be subsequently flowing towards the upper part of the reactor vessel in a region of the baffle blades. From there the polymer suspension flows towards the center part of the reactor vessel. This causes the radial flow of polymer suspension towards the center of the reactor vessel by the action of the baffle blades to be reinforced.
  • a diameter of the stirrer outer circumference is in a range of 50% to 90% of the reactor vessel diameter. In a preferred embodiment the range is 50% to 70% of the reactor vessel diameter. This provides a relatively large stirrer size relative to the reactor vessel diameter, which allows a strong axial flow within the reactor vessel at a relatively low stirrer speed.
  • a distance of at least one stirrer to a lower end of the baffle blades is at least 20% of the reactor vessel height.
  • the reactor vessel has a cylindrical shape.
  • the reactor vessel height is preferably in arrange of 80 to 200 mm. In this range the desired axial flow of polymer suspension near the reactor vessel inner wall is improved.
  • the reactor vessel height is 145 mm and the reactor vessel diameter is 65 mm. With these dimensions improved volumetric gas-liquid mass transfer rate of monomers is achieved.
  • the polymers comprise polyolefins. More preferably the polyolefins comprise polyethylene or polypropylene.
  • the invention also relates to a method of preparing polymers using a reactor as described above.
  • the method comprises stirring a polymer suspension in the reactor vessel with the stirrer, the stirrer is driven at a speed of 1000 rpm or less. In a preferred embodiment the speed is further in a range of 800 - 1000 rpm.
  • Figure 1 shows a cross-section of a reactor according to an embodiment of the invention.
  • Figure 2 shows the reactor according to Figure 1 with an improved stirring effect.
  • Figure 3 shows a top view of the reactor according to Figure 1 with an improved stirring effect.
  • Figure 4 shows a graph of catalytic monomer dissolution of a prior art process.
  • FIG. 1 shows a cross section of a reactor 100 according to an embodiment of the invention
  • the reactor 100 has a reactor vessel 101 , which has preferably vertically extending vessel walls 108 and a bottom. 111 suitable for holding a polymer suspension 106 of a monomer to be polymerized.
  • the reactor vessel 101 can be mounted in a frame (not shown).
  • the reactor 100 can be part of a system of reactors which may be cascaded or arranged in other configurations.
  • a stirrer 102 having at least three, preferably four stirrer blades 104 is placed.
  • the stirrer 102 is attached to a drive shaft 103 which can be driven by a drive 107.
  • the drive 107 can be a controllable electric drive, operable in a speed range from zero to 1000 rpm and more, preferably in a range of 800 - 1000 rpm.
  • baffle is disposed having baffle blades 105 extending from the top of the reactor vessel 112 into the reactor vessel 101.
  • the baffle blades 105 have elongated cross-sections.
  • the baffle blades can be massive but can also have a continuous outer surface enclosing a cavity.
  • the baffle biades 105 can be attached to the reactor vessel wall 108,
  • the baffle blades 105 are preferably attached with one of their ends to a side of the reactor vessel cover 109 that in use of the reactor 100 is arranged to face the interior of the reactor vessel 101. This allows the baffle blades 105 to be extracted from the reactor vessel e.g.
  • the reactor 100 can be provided with input means such as feed lines for introducing the polymer suspension 108 into the reactor vessel 101 and/or output means for extracting the polymer suspension 106 from the reactor vessel 101. Normally the reactor 100. i.e.
  • reactor vessel 101 can also be pressurized.
  • the reactor 100 shown in Figures 1 and 2 has a reactor vessel cover 109 that is provided with a feed line 113 for introducing gaseous chemicals into the reactor vessel 101.
  • Feed line 113 has an outlet 114 that preferably is arranged above the surface 202 of the polymer suspension 106.
  • Figure 2 shows a flow profile 201 of the polymer suspension 106 in a vertical cross section of the reactor 100.
  • the stirrer 102 is arranged to have an axial flow profile 201.
  • the stirrer blades 104 cause the polymer suspension 106 to be pushed downward into the reactor vessel 101 towards the bottom 11 1. Subsequently the polymer suspension flows axially along the reactor vessel wall 108 up towards the surface 202 of the polymer suspension 108 where the polymer suspension 106 assumes a more radial motion towards the center axis of the reactor vessel 101 coinciding with the drive shaft 103.
  • the axial flow profile can be achieved using an axial impeller.
  • Such axial impeller can for example be a propeller type stirrer 102, for example a stirrer having blades 104 with an inclination angle.
  • the stirrer may have 2, 3 or 4 blades.
  • An example of such a stirrer is known as a ViscopropTM stirrer.
  • the correct positioning of the baffle blades relative to the liquid phase surface 202 is preferably to be maintained throughout the polymerization process, as the liquid phase level may vary during the process.
  • the baffle blades 105 are lowered sufficiently deep into reactor vessel 101 , or the polymer suspension surface level relative to the baffle blades 105 when filling the reactor vessel 101 is chosen such that lower portions of the baffle blades 105 extend into the polymer suspension.
  • Figure 3 shows a top view of the reactor vessel 101 where in operation the drive shaft 103 has for example clockwise rotation 301.
  • the reactor 100 is equipped with a baffle 105 having two blades which are positioned opposite to each other in the reactor vessel 101.
  • the polymer suspension shows a rotary flow profile as a consequence of the rotary motion 301 of the stirrer at the bottom 1 11 of the reactor vessel 101 , the polymer suspension will also exhibit a rotary motion component in the same clockwise direction 301 near the reactor vessel wall 108,
  • the baffle blades 105 cause the polymer suspension that rotary flows near the reactor vessel wall 108 to radially flow towards the drive shaft 103, thereby combining the rotary and axial flow profile, see reference numeral 302 in fig, 3.
  • Figure 4 shows a prior art graph of catalytic monomer consumption.
  • the graph shows that after less than 10 minutes a maximum consumption is attained. Gradually in time the consumption rate will drop below.
  • the consumption rate or volumetric gas-liquid mass transfer rate is expressed using the volumetric gas-liquid mass transfer coefficient value 'k L a ⁇ A minimum k L a of 0,03 per second ensures that mass transfer limitations are unlikely to occur, EXPERIMENTS
  • volumetric gas-liquid mass transfer coefficient of ethylene was established in a hexane suspension present in the reactor (Michael Lallemand, "Continuous stirred tank reactor for ethylene oligomerization catalyzed by NiMCM-41 ", CHEMICAL ENGINEERING, ELSEVIER SEQUOIA, LAUSANNE, CH) .
  • -Reactor vessel Cylindrical, 145 mm high, 85 mm diameter
  • -Baffle 2 blades, top mounted, 70-95 mm length, 5 mm baffle width w, 1 mm thickness baffle.
  • Liquid diluent volume 300 mL
  • Table 1 shows that for Stirrer A the coefficient increases to 0,037 1/s. The targeted value of 0,03 1/s is obtained, however a rotation speed of above 500 rpm is not feasible, since at these stirrer speeds, splashing of liquids leads to undestred deposits on the reactor cover and subsequently plugging of the sampling lines for the analytical device.
  • various stirrer designs were tested at a fixed stirrer speed of 800 rpm. The first stirrer which was used was Stirrer A.
  • the second stirrer (Stirrer I) was a propeller type stirrer with double blades
  • the third stirrer (Stirrer II) was a propeller type stirrer with four blades
  • the fourth stirrer (Stirrer III) was a turbine type stirrer having multiple vertical blades (Rushton Turbine)
  • Table 2 below shows the transfer coefficient of this condition for the various stirrer types.
  • Table 3 shows that Stirrer II and baffle combination obtains at 800 rpm a transfer coefficient of 0.041 1/s. This rate is sufficiently above the targeted value of 0,030.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

La présente invention concerne un réacteur pour la préparation de polymères, comprenant : - une cuve de réaction, pour contenir une suspension de polymère, ayant un volume inférieur à 1 l et un rapport de la hauteur au diamètre d'au moins 2 ; - un couvercle de cuve de réacteur comprenant au moins une entrée de ligne d'échantillonnage pour surveiller une composition de phase gazeuse ; - un arbre d'entraînement auquel est fixé au moins un agitateur ayant au moins trois pales d'agitateur positionnées dans une partie inférieure de la cuve de réacteur ; - un dispositif d'entraînement pouvant entraîner l'agitateur à une vitesse de 1000 trs/min ou moins ; - un déflecteur qui est monté par le haut à l'intérieur du couvercle de cuve de réacteur et qui comprend au moins deux pales de déflecteur ayant des sections transversales allongées et ayant des parties inférieures qui s'étendent dans la suspension de polymère jusqu'à un niveau au-dessus de l'au moins un agitateur qui comprend une roue axiale.
PCT/EP2017/058218 2016-04-12 2017-04-06 Réacteur de polymérisation à petite échelle WO2017178323A1 (fr)

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EP16164899.3 2016-04-12
EP16164899 2016-04-12

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110681331A (zh) * 2019-10-15 2020-01-14 老河口新景科技有限责任公司 一种具有壁垢清理装置的反应塔
CN112654424A (zh) * 2018-09-11 2021-04-13 韩华思路信(株) 具有挡板的间歇式反应器
CN113694837A (zh) * 2020-05-21 2021-11-26 中国石油化工股份有限公司 一种用于不饱和聚合物加氢的釜式反应器和方法及一种丁腈橡胶加氢的方法
US11198922B1 (en) 2020-10-29 2021-12-14 Mercury Clean Up, LLC Mercury collection system
CN114392712A (zh) * 2022-02-22 2022-04-26 拓烯科技(衢州)有限公司 一种烯烃模试连续溶液聚合装置和工艺

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002081076A2 (fr) * 2001-04-05 2002-10-17 Symyx Technologies, Inc. Systeme de reacteur chimique combinatoire
EP1310296A2 (fr) * 2000-06-03 2003-05-14 Symyx Technologies, Inc. Réacteurs en parallèle semicontinus ou continus avec un dispositif de pressurisation d'alimentation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1310296A2 (fr) * 2000-06-03 2003-05-14 Symyx Technologies, Inc. Réacteurs en parallèle semicontinus ou continus avec un dispositif de pressurisation d'alimentation
WO2002081076A2 (fr) * 2001-04-05 2002-10-17 Symyx Technologies, Inc. Systeme de reacteur chimique combinatoire

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112654424A (zh) * 2018-09-11 2021-04-13 韩华思路信(株) 具有挡板的间歇式反应器
CN110681331A (zh) * 2019-10-15 2020-01-14 老河口新景科技有限责任公司 一种具有壁垢清理装置的反应塔
CN113694837A (zh) * 2020-05-21 2021-11-26 中国石油化工股份有限公司 一种用于不饱和聚合物加氢的釜式反应器和方法及一种丁腈橡胶加氢的方法
US11198922B1 (en) 2020-10-29 2021-12-14 Mercury Clean Up, LLC Mercury collection system
CN114392712A (zh) * 2022-02-22 2022-04-26 拓烯科技(衢州)有限公司 一种烯烃模试连续溶液聚合装置和工艺

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