WO2004039491A1 - Taylorreaktor für stoffumwandlungen - Google Patents
Taylorreaktor für stoffumwandlungen Download PDFInfo
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- WO2004039491A1 WO2004039491A1 PCT/EP2003/010278 EP0310278W WO2004039491A1 WO 2004039491 A1 WO2004039491 A1 WO 2004039491A1 EP 0310278 W EP0310278 W EP 0310278W WO 2004039491 A1 WO2004039491 A1 WO 2004039491A1
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- rotor
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- taylor
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- reaction volume
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/94—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with rotary cylinders or cones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/50—Pipe mixers, i.e. mixers wherein the materials to be mixed flow continuously through pipes, e.g. column mixers
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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
- B01J19/1806—Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
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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
- 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
- B01J2219/00094—Jackets
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00168—Controlling or regulating processes controlling the viscosity
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/182—Details relating to the spatial orientation of the reactor horizontal
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/187—Details relating to the spatial orientation of the reactor inclined at an angle to the horizontal or to the vertical plane
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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
- 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
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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
- 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
- B01J2219/1946—Details relating to the geometry of the reactor round circular or disk-shaped conical
Definitions
- the present invention relates to a Taylor reactor for physical and / or chemical material conversions, in the course of which an increase in the viscosity of the reaction medium occurs.
- the present invention relates to a new process for converting substances using the Taylor reactor and to the use of the substances produced by the new process.
- Taylor reactors which are used to convert substances under the conditions of the Taylor vortex flow, have long been known. In their original embodiment, they consist of two coaxial, concentrically arranged cylinders, the outer of which is fixed and the inner rotates. The volume that is formed between the inner peripheral surface of the outer cylinder and the outer peripheral surface of the inner cylinder serves as the reaction space. With increasing angular velocity of the inner cylinder, a number of different forms of flow occur, which are characterized by a dimensionless characteristic number, the so-called Taylor number Ta.
- the Taylor number is also dependent on the kinematic viscosity of the fluid in the reaction volume and on the geometric parameters, the outer radius of the inner cylinder R, and the inner radius of the outer cylinder, according to the following formula:
- Rotation speed of the inner cylinder increased further, kick above a critical value, alternately rotating (contrarotating) vortices with axes along the circumferential direction.
- Taylor vortices are rotationally symmetrical, have the geometric shape of a To (Taylor vortex rings) and have a diameter that is approximately as large as the gap width.
- Two adjacent vertebrae form a pair of vertebrae or a vertebral cell.
- This behavior is based on the fact that when the inner cylinder rotates with the outer cylinder at rest, the fluid particles near the inner cylinder are subjected to a stronger centrifugal force than those which are further away from the inner cylinder. This difference in the acting centrifugal forces pushes the fluid particles from the inner to the outer cylinder. The centrifugal force counteracts the viscosity force, since the friction has to be overcome when the fluid particles move. If the speed of rotation increases, then the centrifugal force also increases. The Taylor vortices arise when the centrifugal force becomes greater than the stabilizing viscosity force.
- Taylor reactor If the Taylor reactor is equipped with an inlet and outlet and operated continuously, a Taylor vortex flow with a low axial flow results.
- Each pair of vertebrae moves through the gap, with only a small mass exchange between adjacent pairs of vertebrae.
- the mixing within such vortex pairs is very high, whereas the axial mixing beyond the pair boundaries is only very small.
- a pair of vortices can therefore be regarded as a well-mixed stirred kettle.
- the flow system thus behaves like an ideal flow tube in that the vortex pairs move through the gap with a constant dwell time like ideal stirred tanks.
- the known Taylor reactor is able to essentially solve the problem of maintaining the Taylor flow with a strong increase in the kinematic viscosity v in the reaction medium.
- the reaction volume in the form of an annular gap is defined by the concentrically arranged rotor, the reactor base and the reactor cover.
- the product outlet must be arranged on the side of the Taylor reactor or in the reactor cover and cannot be designed without edges. With this configuration, a trouble-free product outlet can only be implemented with difficulty.
- the known Taylor reactor is not yet capable of all safety and process engineering . Solving problems that occur in bulk polymerization and, on the other hand, it is not yet possible to increase the conversion of the monomers to such an extent that extensive freedom from monomers and a narrow molecular weight distribution and non-uniformity in the molecular weight of the polymers is achieved.
- a Taylor reactor is known from US Pat. No. 4,174,097, in which the rotor is rotatably mounted in the inlet region of the starting materials.
- the rotor is not supported at its other end, but essentially ends in front of the outlet area, which has the same diameter as the outer reactor wall at its widest point.
- the outlet area narrows in a funnel shape to form an outlet pipe.
- the well-known Taylor reactor is used to mix liquids of different viscosities and electrical conductivity. It can also be used to react polysocyanates with polyols. The extent to which it can be used in bulk for the polymerization of olefinically unsaturated monomers is not apparent from the American patent.
- the drive shaft is passed through the reactor floor and the connection to the rotor in the inlet area of the starting materials.
- the ring-shaped reaction volume does not widen in the direction of flow.
- the concentric portions may have configurations other than cylindrical, for example essentially spherical or conical, which configurations are particularly advantageous for bulk polymerization, but will not taught.
- Short-circuit current is thus to be understood as a current inside the reactor in the direction of flow of the reaction media, partially bypassing the mixing process and thus reducing the residence time in the reactor, which leads to lower degrees of polymerization.
- Tests have shown that the Taylor reactor according to the invention is surprisingly suitable for all substance conversions in which. the kinematic viscosity v of the reaction medium changed significantly in the direction of flow.
- the Taylor reactor according to the invention and the process according to the invention allow radical, anionic and cationic (co) polymerization, graft copolymerization and block copolymerization (collectively called “polymerization”) of olefinically unsaturated monomers in bulk with conversions> 70 mol%. It is even more surprising that conversions> 98 mol% can be achieved without problems, without it occurring in the Taylor reactor according to the invention for the formation of disruptive gas bubbles and / or the deposit and of (co) polymers, graft copolymers and block copolymers
- the Taylor reactor according to the invention and the method according to the invention permit particularly reliable reaction control of the polymerization in bulk, which is why the polymers can be prepared very safely, reliably and reproducibly. Due to the very low monomer content of the polymers, they can be used for a wide variety of purposes without further purification, without the occurrence of safety-related, process-related toxicological and ecological problems and unpleasant odors.
- the Taylor reactor according to the invention preferably comprises a reaction volume in the form of an annular gap, which preferably has a circular circumference.
- the ring- gap-shaped reaction volume is defined by or is formed by an outer reactor wall and a rotor arranged concentrically therein, which is arranged rotatably about the axis of rotation.
- the outer reactor wall and the rotor have a circular circumference over the entire length of the reaction volume, as seen in cross section.
- the term "circular” is to be understood as strictly circular, oval, elliptical or polygonal with rounded corners.
- a strictly circular circumference is advantageous for reasons of simplicity of manufacture, simple construction and significantly easier maintenance of constant conditions over the entire length of the annular gap-shaped reaction volume.
- the inner wall of the outer reactor wall and / or the surface of the rotor can be smooth or rough, i.e. the surfaces in question can have a low or high surface roughness. Additionally or alternatively, the inner wall of the outer reactor wall and / or the surface of the rotor can have a relief-like radial and / or axial, preferably radial, surface profile, as described, for example, in US Pat. No. 4,174,907 A or British Pat. GB 1,358,157 becomes. Is a. radial surface profile available, it is advantageously approximately or exactly dimensioned like the Taylor swirl rings.
- the Taylor reactor according to the invention is - viewed in the longitudinal direction - mounted vertically, horizontally or in a position between these two directions. Vertical storage is an advantage. If the Taylor reactor according to the invention is not mounted horizontally, the reaction medium can flow from bottom to top against the force of gravity or from top to bottom with the force of gravity. According to the invention, it is advantageous if the reaction medium 1 is moved against gravity.
- the viscosity development of the reaction medium can be influenced by influencing the flow rate of the reaction medium through the reactor by varying the inflow rate to the inlet.
- the reactor can therefore be used for various reaction mixtures.
- the increase in the cross section of the reaction volume in the flow direction takes place continuously or discontinuously, in particular continuously, according to suitable mathematical functions.
- suitable mathematical functions are straight lines, at least two straight lines that meet at an obtuse angle, parables, hyperbolas, e-functions or combinations of these functions that merge continuously or discontinuously, in particular continuously.
- the mathematical functions are preferably straight lines, that is to say that the preferably annular-shaped cross section of the reaction volume widens more and more constantly in the flow direction in a first section than in a second section in which the cross section increases less, preferably is constant.
- the extent of the increase depends on the expected increase in the viscosity of the reaction medium in the flow direction and can vary from Experts can be estimated using Taylor formula I and / or determined using simple preliminary tests.
- the outer reactor wall can be cylindrical and the rotor can be conical, the rotor having the largest diameter on the inlet side.
- the outer reaction wall may be tapered and the rotor cylindrical, i.e. that its cross-section is constant over the entire rotor length. It is advantageous according to the invention if the outer reactor wall is conical in a first region on the inlet side and cylindrical in a second region and the rotor is cylindrical.
- the outlet arranged axially, i.e. If it opens into the reaction volume in the direction of the axis of rotation of the rotor, the feed of the educts and / or the process substances causes the flow in the reaction volume in the direction of the outlet and through the outlet.
- the flow around the axis of rotation is also used as a driving force for removing the reaction products, in which the outlet opens into the volume of rotation at a radial distance from the axis of rotation.
- the junction can be at any angle between the axis of rotation and the outlet line defined by the outlet. However, it is preferred if the outlet line and the axis of rotation form an angle between 0 ° and 90 °, i.e. the outlet opens into the volume of rotation transversely to the axis of rotation.
- the outlet is approximately perpendicular to the axis of rotation in the confluence area, the proportion of the flow is around the Maximum axis of rotation on the driving force for removing the reaction products. It is then advantageous to design the end adjacent to the outlet in the manner of a pump rotor in order to generate as strong a current as possible about the axis of rotation in this area.
- the inlet for the starting materials, in particular for the olefinically unsaturated monomers, and for suitable process materials, such as catalysts and initiators, above the reactor base.
- the inlet can be arranged on the side or go through the reactor floor.
- the starting materials can be fed to the feed using customary and known methods and devices, such as metering pumps.
- the devices can be equipped with the aid of customary and known mechanical, hydraulic, optical and electronic measuring and control devices.
- one of the mixing devices as described, for example, in German patent application DE 199 60 389 A1, column 4, line 55, to column 5, line 34, can be connected upstream of the feed.
- an outlet area is provided which tapers in the flow direction towards a product outlet.
- the front end of the rotor facing the outlet is designed such that the reaction volume opens into the production process at least substantially free of dead volume.
- the outlet area and the product outlet are defined by the outer reactor wall.
- the tapering of the outlet area can be described by the mathematical functions listed above, with straight lines being preferred. Accordingly, the outlet area preferably tapers conically.
- the front end of the rotor is then preferably conical in order to achieve — as is preferred — that the cross section of the outlet region is essentially constant in the direction of the axis. This has the effect that dead volumes are avoided, but at the same time there is no disadvantageous back pressure.
- the reactor wall in the inlet area, in the area of the annular gap-shaped reaction volume and in the outlet area as well as the inlet or the inlets and the product outlet can be equipped with a heating or cooling jacket, so that they can be heated or cooled in cocurrent or in countercurrent.
- the Taylor reactor according to the invention is customary and known mechanical, hydraulic, optical and electronic measuring and control devices, such as temperature sensors, pressure meters, flow meters, optical or electronic sensors and devices for measuring substance concentrations, viscosities and other physico-chemical variables, which forward their measured values to a data processing system that controls the entire process.
- the Taylor reactor according to the invention is preferably designed to be pressure-tight, so that the reaction medium can preferably be under a pressure of 1 to 100 bar.
- the Taylor reactor according to the invention can consist of a wide variety of materials, as long as these are not attacked by the starting materials and the reaction products and can withstand higher pressures.
- Metals preferably steel, in particular stainless steel, are preferably used.
- the Taylor reactor according to the invention can be used for a wide variety of purposes. It is preferably used for material conversions in which the kinematic viscosity v in the reaction medium increases in the direction of flow.
- Examples of substance conversions that can be carried out in the Taylor reactor according to the invention with particular advantages are the build-up or breakdown of oligomeric and high-molecular substances, such as. B. the polymerization of monomers in bulk, solution, emulsion or suspension or by precipitation polymerization.
- polymer-analogous reactions such as the esterification, amidation or urethanization of polymers which contain side groups which are suitable for such reactions, the preparation of olefinically unsaturated materials which are curable with electron beams or ultraviolet light, the production of polyurethane resins and modified polyurethane resins such as acrylated polyurethanes, the production of (polyJureas or modified (poly) ureas, - the molecular weight build-up of compounds which are associated with
- the process according to the invention is used with very particular advantage for the polymerization of olefinically unsaturated monomers in bulk, because the particular advantages of the Taylor reactor according to the invention are particularly open.
- the Taylor reactor according to the invention is particularly preferably used for the production of chemically uniformly composed polymers and copolymers.
- the more rapidly polymerizing comonomer or the more rapidly polymerizing comonomers can be metered in via feeds arranged one behind the other in the axial direction, so that the comonomer ratio can be kept constant over the entire length of the reactor.
- the Taylor reactor is also used with particular advantage for the graft copolymerization.
- the so-called backbone polymer can be prepared separately and metered into the Taylor reactor according to the invention via a separate feed or in a mixture with at least one monomer.
- the backbone polymer can, however, also be produced in a first section of the Taylor reactor according to the invention, after which at least one monomer which forms the graft branches is metered in via at least one further feed which is offset in the axial direction.
- the monomer or the comonomers can then be grafted onto the backbone polymer in at least one further section of the Taylor reactor according to the invention. If several comonomers are used, they can be metered in individually via one feed or as a mixture through one feed or several feeds. If at least two comonomers are metered in individually and in succession through at least two feeds, it is even possible to produce graft branches, which are block copolymers in their own right, in a particularly simple and elegant manner.
- the production of core-shell latices can be realized particularly simply and elegantly with the help of the Taylor reactor according to the invention.
- the core is first prepared by polymerizing at least one monomer. At least one further comonomer is metered in via at least one further feed and the shell is polymerized onto the core in at least one further section. In this way, several shells can be applied to the core.
- Polymer dispersions can also be prepared with the aid of the Tylor reactor according to the invention.
- at least one monomer in the homogeneous phase, in particular in solution is polymerized in a first section of the Taylor reactor (co) according to the invention, after which a precipitant is metered in via at least one further device, resulting in the polymer dispersion.
- the Taylor reactor according to the invention has the particular advantage of a large specific cooling surface, which allows a particularly reliable reaction to be carried out.
- the Taylor reactor according to the invention is very particularly preferred for the continuous production of (co) polymers, block copolymers and graft copolymers by free radical, anionic or cationic, in particular free radical, (co) polymerization, block mixed polymerization or
- Graft copolymerization of at least one olefinically unsaturated monomer used in bulk by the process according to the invention.
- Suitable monomers which are suitable for the process according to the invention are acyclic and cyclic, optionally functionalized monoolefins and diolefins, vinylaromatic compounds, vinyl ethers, vinyl esters, vinyl amides, vinyl halides, allyl ethers and allyl esters, acrylic acid, and methacrylic acid and their esters, amides and nitriles and maleic acid, Fumaric acid and itaconic acid and their esters, amides, imides and anhydrides.
- maonoolefins examples include ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, cyclobutene, cyclopentene, dicyclopentene and cyclohexene.
- diolefins examples include butadiene, isoprene, cyclopentadiene and cyclohexadiene.
- vinyl aromatic compounds examples include styrene, alpha-methyl styrene, 2-, 3- and 4-chloro, methyl, ethyl, propyl and butyl and tert-butyl styrene and alpha-methyl styrene.
- An example of a suitable vinyl compound or a functionalized olefin is vinylcyclohexanediol.
- Suitable vinyl ethers are methyl, ethyl, propyl, butyl and pentyl vinyl ether, allyl monopropoxylate and trimethylolpropane mono, di and triallyl ether.
- Suitable vinyl esters are vinyl acetate and propionate and the vinyl esters of versatic acid and other quaternary acids.
- Suitable vinylamides are N-methyl-, N, N-dimethyl-, N-ethyl-, N-propyl-, N-butyl-, N-amyl-, N-cyclopentyl- and N-cyclohexylvinylamide as well as N-vinylpyrrolidone and - epsilon-caprolactam.
- Suitable vinyl halides are vinyl fluoride and chloride.
- suitable vinylidene halides are vinylidene fluoride and vinyl chloride.
- Suitable allyl ethers are methyl, ethyl, propyl, butyl, pentyl, phenyl and glycidyl monoallyl ethers.
- Suitable allyl esters are allyl acetate and propionate.
- esters of acrylic acid and methacrylic acid are methyl, ethyl, propyl, n-butyl, isobutyl, n-pentyl, n-hexyl, 2-ethyl-hexyl, isodecyl, decyl and cyclohexyl , t-Butylcyclohexyl, norbonyl, isobornyl, 2- and 3-hydroxypropyl, 4-hydroxybutyl,
- Trimethylolpropane mono-, pentaerythritol mono- and glycidyl (meth) acrylate Trimethylolpropane mono-, pentaerythritol mono- and glycidyl (meth) acrylate.
- di-, tri- and tetra (meth) acrylates of ethylene glycol, di-, tri- and tetraethylene glycol, propylene glycol, dipropylene glycol, butylene glycol, dibutylene glycol, glycerol,
- Trimethylolpropane and pentaerythritol into consideration. However, they are not used alone, but always in minor amounts together with the monofunctional monomers.
- Suitable amides of acrylic acid methacrylic acid are (meth) acrylic acid amide and (meth) acrylic acid-N-methyl-, -N, N-dimethyl-, -N-ethyl-, -N-propyl-, -N-butyl-, -N -amyl-, -N-cyclopentyl- and -N-cyclohexylamide.
- Suitable nitriles are acrylonitrile and methacrylonitrile.
- Maleic acid, fumaric acid and itaconic acid are maleic acid, fumaric acid and itaconic acid dimethyl, diethyl, dipropyl and dibutyl esters, maleic acid, fumaric acid and itaconic acid diamide, Maleic acid, fumaric acid and itaconic acid-N, N 'dimethyl, N, N, N', N ⁇ - tetamethyl-, -N N 'diethyl, N, N', dipropyl, -N , N ' -dibutyl-, -N, N'-diamyl-, - N, N'-dicyclopentyl- and -N, N ' -dicyclohexylamide, maleic, fumaric and itaconic amide and maleic, fumaric and itaconic acid N -methyl-, -N-ethyl-, -N-propyl-, -N-butyl
- the monomers described above can be polymerized by radical, cationic or anionic polymerization. They are advantageously polymerized by free radicals.
- the usual and known inorganic radical initiators or initiators such as
- butyl hydroperoxide e.g. B. tert-butyl perbenzoate, tert.
- 2-ethylhexanoate 2-ethylhexanoate
- Bisazo compounds such as azobisisobutyronitrile
- C-C starters such as 2,3-dimethyl-2,3-diphenyl-butane or hexane
- styrene can also be used, which initiates polymerization thermally even without a radical initiator.
- At least one of the monomers described above is metered in via a lateral inlet into the inlet region of the Taylor reactor according to the invention.
- At least one of the radical initiators or initiators described above is preferably metered in together with at least one monomer via a further side feed.
- the monomer or monomers are at least partially polymerized in the reaction volume under the conditions of the Taylor flow.
- the resulting liquid polymer is conveyed from the reaction volume in the form of an annular gap into the outlet area and from there into the product outlet and discharged via the pressure-maintaining valve.
- the conditions for the Taylor flow are preferably met in part of the annular gap-shaped reaction volume or in the entire annular gap-shaped reaction volume, in particular in the entire annular gap-shaped reaction volume.
- the temperature of the reaction medium can vary widely in the process according to the invention and depends in particular on the monomer with the lowest decomposition temperature, on the temperature at which the depolymerization begins, and on the reactivity of the monomer or monomers and the initiators.
- the polymerization is preferably carried out at temperatures from 100 to 200, preferably 130 to 180 and in particular 150 to 180 ° C.
- the polymerization can be carried out under pressure.
- the pressure is preferably 1 to 100, preferably 1 to 25 and in particular 1 to 15 bar.
- the throughput time can vary widely and depends in particular on the reactivity of the monomers and the size, in particular the length, of the Taylor reactor according to the invention.
- the throughput time is preferably 15 minutes to 2 hours, in particular 20 minutes to 1 hour.
- conversions> 80, preferably> 90, particularly preferably> 95, very particularly preferably> 98 and in particular> 98.5 mol% can be achieved without problems.
- the kinematic viscosity v can increase at least tenfold, in particular at least a hundredfold.
- the molecular weight of the polymers prepared using the process according to the invention can vary widely and is essentially limited only by the maximum kinematic viscosity v at which the Taylor reactor according to the invention can maintain the conditions of the Taylor flow.
- the number average molecular weights of the polymers prepared in the process according to the invention are preferably 800 to 50,000, preferably 1,000 to 25,000 and in particular 1,000 to 10,000 Daltons.
- the non-uniformity of the molecular weight is preferably ⁇ 10, in particular ⁇ 8.
- Fig. 1 schematically - an embodiment of a Taylor reactor according to the invention according to the first alternative of the invention in longitudinal section;
- Fig. 2 shows another embodiment of an inventive Taylor reactor according to the first alternative of the invention in one
- FIG. 1 corresponding representation
- 3 shows an embodiment of a Taylor reactor according to the invention in accordance with the second alternative of the invention in a view corresponding to FIG. 1;
- Fig. 4 shows an embodiment of a Taylor reactor according to the invention, in which both alternatives of the invention are implemented, in a view corresponding to Fig. 1 and 2.
- Fig. 5 shows an embodiment of a Taylor reactor according to the invention according to the third alternative of the invention in a view corresponding to Fig. 1 and
- FIG. 6 shows a section along section line VI - VI in FIG. 5
- the Taylor reactor designated 100 as a whole in FIG. 1 comprises a reactor housing 103, the lower region of which, as shown in FIG. 1, which corresponds to the normal operating position of the Taylor reactor 100, is designed as an application region 108.
- the part 103.2 of the reactor housing 103 adjoining the inlet region 108 is designed to widen conically up to the point 103.3, so that the cross section of the reaction volume 102 increases in the part 103.2.
- a cylindrical part 103.4 of the reactor housing 103 which extends beyond the upper end face 104.2 of the rotor 104.
- the cylindrical part 103.4 is followed by a funnel-shaped outlet area 109 which opens into an outlet 110 which serves to discharge the reaction products.
- the outlet 110 is a
- Pressure-maintaining valve 111 is connected downstream, with which the reaction media in the reaction volume can be kept under a predeterminable pressure.
- the rotor 104 is mounted rotatably about an axis A on the inlet-side end wall 105 shown in FIG. 1 below.
- a drive shaft 107 which is passed through the end wall 105 and is connected to a rotary drive (not shown in the drawing), for example an electric motor, is used to introduce a torque causing the rotation into the rotor 104.
- the sealing of the reaction volume 102 in the area of the passage of the drive shaft 107 through the end wall 105 is provided by a mechanical seal 106 which is arranged between the end 104. 1 of the rotor 104 shown in the drawing below and the end wall 105.
- one or more inlets can be equipped with mixing devices 112.
- the design of the reactor housing 103 and the rotor 104 has the effect that the cross section of the reaction volume in the reactor housing part 103.2, seen from the inlet to the outlet, initially increases, but the increase from the point 103.3, however, in the exemplary embodiment illustrated to the Value 0 - decreases to the outlet in the cylindrical housing part 103.4.
- FIG. 2 The exemplary embodiment shown in FIG. 2 is largely identical in its technical configuration with that according to FIG. 1 match. In order to avoid repetitions, only the differences will be explained below. Components corresponding to the exemplary embodiment from FIG. 1 are provided with reference numerals increased by 100.
- the reactor housing 203 is designed to widen conically up to the outlet region 209.
- the rotor 204 which is cylindrical in the lower region according to FIG. 2, has a point 204.3 from which it merges into a region 204.4 which widens conically towards the outlet region 209.
- the taper corresponds to that of the reactor housing 203, so that the cross section of the reaction volume remains constant from the point 204 to the upper end of the rotor.
- the reactor housing 303 of the Taylor reactor 301 is designed to widen conically from the inlet region 308 to the outlet region 309.
- the rotor 304 has a cylindrical shape which merges into a cone 313 at the point 304.3.
- the cone angle d is selected such that the cone surface 314 runs parallel to the wall 303.4 of the reactor housing 303 delimiting the outlet region 309. In this way it is achieved that the reaction volume. opens into the outlet 310 at least substantially free of dead volume. This will take effect avoided that 304 parts of the reaction medium are deposited above the rotor, which would lead to an undesired further polymerization by extending the residence time in the reactor.
- Fig. 4 shows a particularly preferred embodiment of a Taylor reactor according to the invention, in which both alternatives of the invention are realized.
- the Taylor reactor now designated 401, comprises a reactor housing 403 which corresponds to that shown in FIG. 1.
- the rotor 404 - like that in FIG. 3 - is provided with a cone 413 at its upper end.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
- Polymerisation Methods In General (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003283244A AU2003283244A1 (en) | 2002-10-30 | 2003-09-16 | Taylor reactor for substance transformation |
JP2004547490A JP4718185B2 (ja) | 2002-10-30 | 2003-09-16 | 物質変換のためのテイラー反応器 |
US10/531,334 US20060062702A1 (en) | 2002-10-30 | 2003-09-16 | Taylor reactor for substance tranformation |
EP03775153A EP1558375A1 (de) | 2002-10-30 | 2003-09-16 | Taylorreaktor f r stoffumwandlungen |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10250420.2 | 2002-10-30 | ||
DE10250420A DE10250420A1 (de) | 2002-10-30 | 2002-10-30 | Taylorreaktor für Stoffumwandlungen |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004039491A1 true WO2004039491A1 (de) | 2004-05-13 |
Family
ID=32185284
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2003/010278 WO2004039491A1 (de) | 2002-10-30 | 2003-09-16 | Taylorreaktor für stoffumwandlungen |
Country Status (6)
Country | Link |
---|---|
US (1) | US20060062702A1 (de) |
EP (1) | EP1558375A1 (de) |
JP (1) | JP4718185B2 (de) |
AU (1) | AU2003283244A1 (de) |
DE (1) | DE10250420A1 (de) |
WO (1) | WO2004039491A1 (de) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005085304A1 (en) | 2004-03-01 | 2005-09-15 | Bridgestone Corporation | Continuous polymerization reactor |
DE102007021012A1 (de) | 2007-05-04 | 2008-11-06 | Basf Coatings Ag | Kontinuierliches Polymerisationsverfahren zur Erzeugung von Polymeren mit enger Molmassenverteilung und Taylor-Couette-Reaktor für seine Durchführung |
DE102007050284A1 (de) | 2007-10-18 | 2009-04-23 | Evonik Röhm Gmbh | Verfahren zur Amidierung von Nitrilen in Gegenwart von Schwefelsäure |
Families Citing this family (11)
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DE10149015B4 (de) * | 2001-10-04 | 2005-04-14 | Basf Coatings Ag | Verfahren zur kontinuierlichen Polymerisation in Masse und Taylorreaktor für seine Durchführung |
ATE531743T1 (de) * | 2008-08-08 | 2011-11-15 | Constr Res & Tech Gmbh | Herstellung von silylierten polyurethanen und/oder polyharnstoffen |
US7964301B2 (en) * | 2009-06-26 | 2011-06-21 | Global Energy Science, LLC (California) | Dynamic accelerated reaction batteries utilizing Taylor Vortex Flows |
JP5131871B2 (ja) * | 2010-05-10 | 2013-01-30 | 丸井 智敬 | 被プロセス材および微小気泡を混相流としてプロセスを行う装置 |
US8158277B1 (en) * | 2010-09-30 | 2012-04-17 | Global Energy Science, LLC (California) | Cross-flow electrochemical batteries |
EP2810706B1 (de) * | 2012-02-01 | 2024-08-14 | LG Energy Solution, Ltd. | Reaktor zur herstellung eines vorläufers von lithium-verbund-übergangsmetalloxid und verfahren zur herstellung |
KR101424610B1 (ko) | 2013-06-14 | 2014-08-04 | (주) 라미나 | 코어-쉘 입자 제조장치 및 이를 이용한 코어-쉘 입자 제조방법 |
KR20150109757A (ko) * | 2014-03-20 | 2015-10-02 | 고려대학교 산학협력단 | 금속 분말의 제조 방법 및 이를 구현하는 금속 분말의 제조 장치 |
WO2018001474A1 (de) | 2016-06-29 | 2018-01-04 | Wacker Chemie Ag | Verfahren zur herstellung von vinylacetat-ethylen-copolymerisaten mittels emulsionspolymerisation |
KR102097584B1 (ko) * | 2018-05-04 | 2020-04-06 | 재단법인 차세대융합기술연구원 | 지속적으로 테일러 유동을 유지 가능한 테일러 반응기 |
KR102176625B1 (ko) * | 2018-11-30 | 2020-11-09 | (주)포스코케미칼 | 선속도 및 유체의 진행 방향이 가변적인 반응기 |
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2003
- 2003-09-16 WO PCT/EP2003/010278 patent/WO2004039491A1/de active Application Filing
- 2003-09-16 EP EP03775153A patent/EP1558375A1/de not_active Withdrawn
- 2003-09-16 US US10/531,334 patent/US20060062702A1/en not_active Abandoned
- 2003-09-16 AU AU2003283244A patent/AU2003283244A1/en not_active Abandoned
- 2003-09-16 JP JP2004547490A patent/JP4718185B2/ja not_active Expired - Fee Related
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GB615425A (en) * | 1945-07-30 | 1949-01-06 | James George Fife | Improvements in method of contacting fluids one with another |
US3926654A (en) * | 1970-04-03 | 1975-12-16 | Agfa Gevaert | Method of preparing a polyphase system |
DE3327137A1 (de) * | 1982-08-05 | 1984-02-09 | Konishiroku Photo Industry Co., Ltd., Tokyo | Verfahren zur herstellung von fluessigen teilchen einer dispergierten loesung |
DE19828742A1 (de) * | 1998-06-27 | 1999-12-30 | Basf Coatings Ag | Taylorreaktor für Stoffumwandlungen, bei deren Verlauf einer Änderung der Viskosität v des Reaktionsmediums eintritt |
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WO2003031056A1 (de) * | 2001-10-04 | 2003-04-17 | Basf Coatings Ag | Verfahren zur kontinuierlichen polymerisation in masse und taylorreaktor für seine durchführung |
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WO2005085304A1 (en) | 2004-03-01 | 2005-09-15 | Bridgestone Corporation | Continuous polymerization reactor |
US7442748B2 (en) | 2004-03-01 | 2008-10-28 | Bridgestone Corporation | Continuous polymerization reactor |
DE102007021012A1 (de) | 2007-05-04 | 2008-11-06 | Basf Coatings Ag | Kontinuierliches Polymerisationsverfahren zur Erzeugung von Polymeren mit enger Molmassenverteilung und Taylor-Couette-Reaktor für seine Durchführung |
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Also Published As
Publication number | Publication date |
---|---|
DE10250420A1 (de) | 2004-09-16 |
JP4718185B2 (ja) | 2011-07-06 |
US20060062702A1 (en) | 2006-03-23 |
EP1558375A1 (de) | 2005-08-03 |
JP2006504513A (ja) | 2006-02-09 |
AU2003283244A1 (en) | 2004-05-25 |
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