EP3325121A1 - Colonne de traitement thermique de mélanges fluides, contenant notamment des monomères (méth)acryliques - Google Patents

Colonne de traitement thermique de mélanges fluides, contenant notamment des monomères (méth)acryliques

Info

Publication number
EP3325121A1
EP3325121A1 EP16736065.0A EP16736065A EP3325121A1 EP 3325121 A1 EP3325121 A1 EP 3325121A1 EP 16736065 A EP16736065 A EP 16736065A EP 3325121 A1 EP3325121 A1 EP 3325121A1
Authority
EP
European Patent Office
Prior art keywords
column
nozzle
liquid
mass transfer
cavity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP16736065.0A
Other languages
German (de)
English (en)
Inventor
Ulrich Hammon
Thomas Walter
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of EP3325121A1 publication Critical patent/EP3325121A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/26—Fractionating columns in which vapour and liquid flow past each other, or in which the fluid is sprayed into the vapour, or in which a two-phase mixture is passed in one direction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/324—Tray constructions
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment

Definitions

  • the present invention relates to a column for the thermal treatment of fluid mixtures. It has a cylindrical, vertically oriented column body which forms a column cavity and a vertical inner surface. The column further comprises a plurality of column cavities mounted vertically spaced from each other. Furthermore, the column comprises at least one stub which is arranged in the column body and which extends away from the column body, and a closable access opening, which is formed at the stub.
  • the column is in particular a separation column. Furthermore, the invention relates to a thermal separation process between at least one gas rising in a column and at least one liquid descending in the column.
  • gaseous (ascending) and liquid (descending) streams are often passed in countercurrent, with at least one of the streams containing in particular a (meth) acrylic monomer.
  • a heat and mass transfer takes place, which ultimately causes the separation (or separation) desired in the separation column.
  • separation processes should be referred to as thermal separation processes.
  • thermal separation processes examples are the fractionating condensation (cf., for example, DE 19924532 A1, DE 10243625 A1 and WO 2008/090190 A1) and the rectification (in both cases the ascending vapor phase is in countercurrent to descending
  • the separation effect is due to the fact that the vapor composition is different in equilibrium from the liquid composition), the absorption (at least one ascending gas is led to at least one descending liquid in countercurrent, the separation effect is based on the different solubility of the gas components in the Liquid) and desorption (the reverse process for absorption; the liquid dissolved in the liquid phase is separated by partial pressure reduction; the partial pressure reduction of the liquid phase solute is at least partially characterized by passing a carrier gas through the liquid phase et this thermal separation process as stripping; alternatively or additionally (at the same time as a combination), the partial pressure reduction can be effected by lowering the working pressure).
  • the separation of (meth) acrylic acid or (meth) acrolein from the product gas mixture of the catalytic gas phase oxidation can be carried out so that the (meth) acrylic acid or the (meth) acrolein by absorption into a solvent (eg water or an organic solvent ) or by fractionation-forming condensation of the product gas mixture is first separated in bulk and the resulting absorbate or condensate is subsequently further separated to give more or less pure (meth) acrylic acid or (meth) acrolein (cf., for example, DE-10332758 A1, DE No.
  • a solvent eg water or an organic solvent
  • acrylic monomers in this document is abbreviated to "acrylic monomers and / or methacrylic monomers".
  • acrylic monomers is used in this document to shorten “acrolein, acrylic acid and / or esters of acrylic acid”.
  • methacrylic monomers is used in this document to shorten “methacrolein, methacrylic acid and / or esters of methacrylic acid”.
  • the (meth) acrylic monomers mentioned in this specification are to comprise the following (meth) acrylic esters: hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, glycidyl acrylate, glycidyl methacrylate, methyl acrylate, methyl methacrylate, n-butyl acrylate, isobutyl acrylate, isobutyl Butyl methacrylate, n-butyl methacrylate, tert-butyl acrylate, tert-butyl methacrylate, ethyl acrylate, ethyl methacrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate, N, N-dimethylaminoethyl acrylate and N, N-dimethylaminoethyl methacrylate.
  • (Meth) acrylic monomers are important starting compounds for the preparation of polymers which are e.g. be used as adhesives or as water super absorbent materials in hygiene articles use.
  • (meth) acrolein and (meth) acrylic acid are predominantly produced by catalytic gas-phase oxidation of suitable C3 / C4 precursor compounds (or precursors thereof).
  • suitable C3 / C4 precursor compounds or precursors thereof.
  • propene and propane are preferably used as such precursor compounds.
  • methacrylic acid and methacrolein iso-butene and iso-butane are the preferred precursor compounds.
  • suitable starting materials are, however, other compounds containing 3 or 4 carbon atoms, for example isobutanol, n-propanol or precursor compounds thereof, for example the methyl ether of isobutanol.
  • Acrylic acid can also be produced by gas-phase catalytic oxidation of acrolein.
  • Methacrylic acid can also be produced by gas-phase catalytic oxidation of methacrolein.
  • product mixtures are normally obtained from which the (meth) acrylic acid or the (meth) acrolein must be separated off.
  • Esters of (meth) acrylic acid are e.g. by direct reaction of (meth) acrylic acid and / or (meth) acrolein with the corresponding alcohols.
  • product mixtures are first of which make up the
  • the separation columns in which these separation processes are carried out contain separating internals. These pursue in the thermal separation process the purpose of increasing the surface area for the separation in the separation column causing heat and mass transfer ("the exchange surface").
  • the separation columns used are those which contain at least one sequence of mass transfer trays, at least as part of the separating internals.
  • Mass transfer trays pursue the purpose of providing areas in the separation column in the form of liquid layers which form on them, with substantially closed liquid phases.
  • the surface of the vapor or gas stream rising in the liquid layer and thereby dispersing in the liquid phase is then the relevant exchange surface.
  • a succession of mass transfer trays is understood to mean a succession (one after the other) of at least two superimposed in the separation column, generally identically constructed (ie, identical) mass transfer trays.
  • the clear distance between two mass transfer trays directly following one another in such a series (series) of mass transfer trays is made uniform (ie, the mass transfer trays are arranged equidistantly one above the other in the separation column).
  • the simplest embodiment of a mass transfer tray is the so-called Regensiebêt.
  • the cross section of the passages of a dual-flow tray is adapted in a conventional manner its load. If it is too small, the ascending gas flows through the passage openings at such a high speed that the liquid descending in the separation column is entrained substantially without separation effect. If the cross section of the passages is too large, ascending gas and descending liquid move past one another substantially without replacement, and the mass transfer tray runs the risk of running dry.
  • the separating effective working area of a Regensiebêts (dual-flow floor) has two limits.
  • a minimum limiting speed of the ascending gas must be present in order to keep a certain liquid layer on the rain sieve bottom, in order to enable a segregation work of the rain sieve bottom.
  • the upper limit of the velocity of the rising gas is determined by the flood point, when the gas velocity leads to congestion of the liquid on the Regensiebêt and their rain is prevented.
  • Passage point lying points is typically 10 to 80 mm (see, for example, DE 10156988 A1).
  • the passages within a rain screen are identical (ie, they all have the same geometric shape and cross section (cross sectional area)). In terms of application, its cross-sectional areas are circles. That is, preferred Passage openings of rain screen floors are circular holes.
  • the relative arrangement of the passage openings of a Regensiebêts advantageously follows a strict triangular division (see, for example, DE 10230219 A1). Of course, the passages within one and the same Regensiebêts also different borrowed be designed (vary over the Regensiebêt).
  • a sequence of rain sieve bottoms in a separation column comprises identical (identical) rain sieve trays, which are preferably arranged equidistantly one above the other.
  • each dual-flow bottom of a corresponding bottom sequence concludes flush with the wall of the separation column.
  • a rain sieve bottom usually still has at most openings which serve to fasten the floor to support rings or the like (cf., for example, DE 10159823 A1).
  • the liquid descending in the separation column is raining in drops from dual flow soil to dual flow soil, i.e., the gas phase rising between the dual flow trays is permeated by a divided liquid phase.
  • the falling on the respective bottom Regensiebêt drops are partially sprayed on impact.
  • the gas stream flowing through the passage openings bubbles through the liquid layer formed on the surface of the floor, whereby an intensive mass and heat exchange takes place between the liquid and the gas.
  • Dual-flow trays suitable for the purposes of this document are e.g. in Technical Progress Reports, Vol. 61, Fundamentals of the Dimensioning of Column Trays, pages 198 to 21 1, Verlag Theodor Steinkopf, Dresden (1967) and described in DE 10230219 A1.
  • sequences of mass transfer trays are distinguished with such forced liquid trays.
  • mass transfer trays are characterized in that, in addition to the passages already described, they additionally have at least one downcomer.
  • This is at least one drainage opening located in the mass transfer tray, which retains the liquid (eg, a drain weir (this may in the simplest embodiment extend the drain opening with a throat (a chimney, in the case of a circular drain opening of a tube) above)), and which discharges into a passage which runs down to the mass transfer tray below, which as a rule is centrally symmetrical with respect to an axis pointing in the column longitudinal direction.
  • the cross-section of the well may vary along this axis (e.g., taper) or be constant.
  • the liquid descending from a higher mass transfer tray can, independently of the gas or vapor rising through the passages of this mass transfer tray as at least one feed of liquid to the next lower mass transfer tray within a sequence of such mass transfer trays descend the sequence.
  • Such a hydraulic lock can e.g. can be achieved by pulling the downcomer downwards (so far downwards) that it dives deep enough into the liquid layer located on the next lower mass transfer tray of the sequence (such a closure is also referred to in this document as " static closure ").
  • the liquid level required for this purpose can be determined on the lower mass transfer tray, e.g. be ensured by the height of appropriate weirs.
  • the "inflow area" of the at least one downcomer on the mass transfer tray below may also have through openings, thus increasing the available exchange area of the mass transfer tray, and thus its separating effect.
  • a static fluid closure of the downcomer can be effected in this case, for example, by means of a mounted below the outlet end of the downcomer collecting cup.
  • the jacket wall of the collecting cup is pulled up so far that the outlet end of the downcomer dips into the collecting cup (it is also possible to allow the bottom edge of the downcomer to end at the upper edge of the collecting cup).
  • the liquid flowing down through the downcomer accumulates in the collecting cupboard until it reaches above the upper edge of the shell wall of the collecting tray. se drains off.
  • the lower edge of the downcomer dips into the liquid in the collecting cup and the collecting cup forms a siphon-like liquid cap of the downcomer.
  • a raised drainage shaft can also be closed dynamically.
  • the downcomer can be closed, for example, at its lower end with a bottom, which is provided with outlet openings which are dimensioned such that the liquid accumulates in the downcomer and the penetration of gas is prevented (cf., for example, EP 0882481 A1 and DE 10257915 A1 ).
  • the shaft closure is produced dynamically by the pressure loss that arises at the outlet openings.
  • the closure of the drainage shaft is characterized in that its outlet end immersed in jammed liquid, and dynamic closure effect constructive features at the outlet end of the downcomer that the exiting (leaking) liquid suffers a pressure loss in the downcomer backlog in selbigem descending liquid causes, which causes the closure.
  • a pressure loss can be caused by the fact that one selects the cross section of the outlet opening of the downcomer small compared to the average cross section of the shaft.
  • the execution of the at least one downcomer is relevant.
  • the cross-section of the at least one downcomer must be sufficiently large (usually the corresponding cross-sectional area is greater than the cross-sectional area of a passage opening), so that the liquid can safely descend through the at least one downcomer even at the maximum load of the separation column does not back up to the overlying ground.
  • it must be ensured that the hydraulic closure of the at least one downcomer still exists even with minimal liquid load.
  • a favorable flow rate of the liquid accumulated in the downcomer out of the downcomer in the method according to the invention is, for example, 1.2 m / s.
  • Such a liquid guide on a mass transfer tray within a sequence of identical mass transfer trays shall be referred to herein as a cross flow, the sequence of such identical mass transfer trays as a succession of equivalent crossflow mass transfer trays and the single mass transfer tray within the sequence as cross flow mass transfer trays.
  • the cross-flow mass transfer tray is a cross-flow sieve tray.
  • the at least one downcomer Apart from the at least one downcomer, it has passage openings for the gas rising in a separating column, for the design of which basically all the embodiments mentioned in the rain screen floor come into consideration.
  • a cross-flow sieve bottom as through-openings also has circular bores which, in terms of application technology, advantageously also have a uniform radius.
  • the at least one downcomer makes it possible for the liquid descending in a separation column to pass through a succession of crossflow trays independently of the flow path of the successive rising vapor (through the passage openings) from a higher crossflow sieve tray to the next descend lower-lying cross-flow sieve tray can.
  • the liquid flows in cross-flow from the at least one inlet of the lower floor formed by the at least one outlet of the higher cross-sieve tray to the at least one downcomer (to the at least one drain) of the lower floor, e.g. the height of at least one drain weir, via which the liquid can flow to the at least one downcomer, ensures the desired liquid level on the lower cross-flow sieve bottom.
  • the at least one inlet of the lower floor formed by the at least one outlet of the higher cross-sieve tray to the at least one downcomer (to the at least one drain) of the lower floor, e.g. the height of at least one drain weir, via which the liquid can flow to the at least one downcomer, ensures the desired liquid level on the lower cross-flow sieve bottom.
  • the gas streams (vapor streams) emerging from neighboring hoods which are preferably distributed equidistantly over the trays, swirl the liquid accumulated on the bottom and form a bubbling layer in the same, in which the material and heat exchange takes place.
  • Such cross-flow mass transfer trays are also referred to as cross-flow bubble trays or cross-flow tray trays. Since they also contain liquid accumulated with low rising gas (vapor) and thus run the risk of running dry, they are also referred to as hydraulically sealed cross flow trays. In comparison to cross-flow sieve trays, they usually require higher investment costs and cause higher pressure losses of the gas rising through them. In contrast to the simple sieve passage opening of a sieve tray, the through-opening of these trays, which is designed as described, is also referred to as bell passage opening or hood passage opening.
  • the most important component of the cross-flow bubble tray is the bell (cf., for example, DE 10243625 A1 and Chemie-Ing.-Techn. 45th 1967 / No. 9 + 10, pages 617 to 620).
  • the bells (Dampfumlenkhauben, hoods) distinguishes cross flow bell bottoms z.
  • the cross-sections of the passage opening, chimney (neck) and bell (steam deflection hood) are round (eg the cylinder bell bottom or the flat bubble bottom), tunnel cross flow trays (the cross sections of the passage opening, chimney and bell ( Hood) are rectangular, the passage points with their bells are arranged within juxtaposed rows one behind the other, wherein the longer rectangular edge is aligned parallel to the transverse flow direction of the liquid) and cross-flow
  • Thormann ® floors (the cross-sections of the passage opening, chimney and bell (hood) are rectangular, the passage points with their bells are arranged within juxtaposed rows one behind the other, with the longer rectangular edge is aligned perpendicular to the cross-flow direction of the liquid).
  • Cross-flow Thormannböden are z.
  • the bell edge can have very different shapes in the case of crossflow bubble trays (compare DE 10243625 A1 and Chemie-Ing. Techn. 45th 1967 / No. 9 + 10, pages 617 to 620).
  • Figure 3 from Chemie-Ing. Techn. 45 years. 1973 / No. 9 + 10, p. 618 shows some examples of the serrated and slotted edge.
  • the serrations and slots are usually shaped so that the steam entering the mass stored on the mass transfer tray out of the bell dissolves as easily as possible into a large number of bubbles or jets of steam.
  • FIG. 3 and various figures of DE 10243625 A1 also show exemplary embodiments of bell edges, which have a sawtooth-like structure whose teeth are additionally equipped with guide vanes (guide surfaces) ("bent-slots").
  • the guide vanes are to impose a tangential exit direction on the gas stream (vapor stream) emerging from the bent sawtooth-like slots (direct the gas exit into the liquid in an oblique direction), whereby the surrounding liquid receives a directed impulse of movement, which interacts with the arrangement of the bells (steam deflection hoods). can result in a directional liquid flow on the cross-flow bubble tray overlaying the cross-flow established across the mass transfer tray (often such upturned slots are also referred to as drive slots).
  • the liquid does not flow on a lower cross-flow Thormann bottom directly across the ground, but driven in a manner described above, meandering from the at least one inlet to the at least one drain.
  • the details of a cross-flow Thormann convinceds also usually takes place so that the liquid flows in two in the cross-flow direction respectively successive grooves in countercurrent (see, for example, Figure 3 DE 10243625 A1).
  • the resulting meandering of the cross-flow extends the flow path of the liquid from the at least one inlet to the at least one drain, which favors the separation effect of a cross-flow Thormann convinceds.
  • cross-flow mass transfer tray As a valve (as a valve passage opening).
  • the resulting cross-flow mass transfer trays are referred to as cross-flow valve trays (see, for example, DD 279822 A1, DD 216633 A1 and DE
  • cross-flow valve floors subsumes in this document thus cross-flow mass transfer trays, the passage openings (bottom holes) with stroke-limited plate, ballast or lifting valves (floating flaps) that adjust the size of the steam passage opening of the respective column load.
  • the passage openings of the floor for the aforementioned purpose are covered with upwardly movable lids or plates (disks).
  • the lids plates, disks
  • the lids are raised by the gas flow in an additionally via the respective passage opening mounted (which is usually firmly anchored to the ground) corresponding guide frame (guide cage) and finally reach a gas load corresponding lifting height (instead of Guide cage, the disc can also have anchored with the floor upwardly movable valve legs whose upward mobility is limited upwards).
  • the ascending through the passage opening gas flow is deflected at the bottom of the raised lid (plate, disc) in a similar manner as in the bell (at a bell passage opening) and emerges from the under the raised plate (lid, disc) resulting emergence area and as in the Bubble tray parallel to the bottom into the liquid stored on it.
  • the plate stroke thus controls the size of the gas outlet area and adapts itself to the column load until the upper end of the guide cage limits the maximum possible lifting height.
  • the plates may have downwardly directed spacers, so that at low gas load, the valve closes only so far that created by the spacers space still allows intensive mixing of the horizontal gas outflow with the cross-flow liquid. Spacers also counteract adhesion of the valve disc on the ground.
  • valve elements of a cross-flow valve bottom By suitable design of the valve elements of a cross-flow valve bottom, the blowing direction of the valve element can be adjusted and thus the forced liquid flow on the cross-flow valve bottom can be additionally influenced (cf., for example, DD 216 633 A1).
  • the principle of cross-flow valve trays and usable for the purposes of the present document valve bottoms is found, for. B. in Technical Progress Reports, Volume 61, Basics of Dimensioning Column Trays, page 96 to 138 executed.
  • the expert In addition to the above-described movable valves, the expert also knows fixed valves. These are usually disc-shaped, or trapezoidal or rectangular units punched out of the bottom plate and connected thereto via upstanding fixed legs.
  • the bell size can be changed in cross-flow bubble trays or by using z. B. plates (lids) with different weight in cross-flow valve floors can be compensated in this regard, so that the Stoffaus- exchange floor over its cross-section substantially uniform guest (where the liquid level is smaller on the cross-flow mass transfer tray, the seat height of the bell
  • the seat height of the bell can also be lowered, for example, by lowering the length of the corresponding chimney, at the end of which the bell is optionally screwed, in a targeted manner
  • the serration / slot structure of the bell rim may also be varied to provide the desired flow resistance compensation, ideally, adjustment via the crossflow mass transfer tray is such that, during operation of the separation column, each of the units located on a crossflow bell oden located bell caused the same flow resistance for the rising gas).
  • the passage points (the passage openings) of a cross-flow mass transfer tray are generally designed advantageously uniform.
  • the cross-sectional area is usually more than 200 times smaller than the total cross-sectional area of all other openings of the Querstromstoff headboden (the cross section of the at least one downcomer not included) form no (effective) Passage openings for the gas rising through the crossflow mass transfer tray and are therefore not attributed to the same.
  • such openings may be tiny idle bores through which hydraulically sealed crossflow trays may run empty when a separation column is switched off. Also, such openings can serve Verschraubungs- purposes.
  • the prior art recommends the use of sequences of at least two identical (identically designed) cross-flow mass transfer trays u. a. separation columns containing separating internals which are used to carry out thermal separation processes between at least one gas stream rising in the separation column and at least one liquid stream descending in the separation column, and wherein at least one of the streams contains at least one (meth) acrylic monomer.
  • DE 19924532 A1, DE 10243625 A1 and WO 2008/090190 A1 recommend the use of a sequence of structurally identical hydraulically sealed crossflow mass transfer trays in a separation column for carrying out a fractional condensation process of a product gas mixture comprising acrylic acid of a heterogeneously catalyzed gas phase partial oxidation C3 precursors of acrylic acid with molecular oxygen containing from bottom to top first dual-flow trays and then hydraulically sealed cross-flow mass transfer trays.
  • the invention particularly relates to columns in which the aforementioned trays are used.
  • a problematic property of (meth) acrylic monomers is their tendency to undesired polymerization, which, especially in the liquid phase, can not be completely suppressed even by the addition of polymerization inhibitors.
  • a disadvantage of known separation columns is that, when the thermal separation process is carried out continuously over a longer period of operation, the mass transfer trays are comparatively frequently used to form unwanted polymer. This is particularly disadvantageous because the operator of the thermal separation process due to the unwanted Polymerisataise must interrupt the thermal separation process again and again to remove the polymer formed. The same can indeed partially or completely close the passages of the mass transfer tray.
  • radical polymerization of (meth) acrylic monomers is usually highly exothermic, i. H. under strong heat. There is a risk that the polymerization proceeds so vigorously that the separation column containing the polymerization mixture explodes.
  • inspection openings are provided in the column body.
  • Such an inspection opening is formed for example in a nozzle which is arranged in the column body.
  • the diameter of the inspection opening is adapted to the intended function of the inspection opening. It may be a so-called hand hole, through which a person can insert their hand, for example, together with a cleaning device.
  • the inspection opening can be designed as a manhole, in which the diameter of the opening is so large that in non-operation, a worker can get into the cavity of the columns to perform there inspection and cleaning.
  • the polymerizate of the acrylic acid which has been formed in an undesired manner during operation of the column can also be removed via the inspection opening.
  • the floors mounted in the column cavity are usually arranged so that the inspection opening is located between two floors.
  • the inspection opening is designed as a manhole, this has the disadvantage that the distance between the floors is undesirably large. If no separation-effective internals are provided in the area of the inspection opening, unwanted polymer can form in this area.
  • a column for the thermal treatment of fluid mixtures comprising a cylindrical, vertically oriented column body forming a column cavity and a vertical inner surface, a plurality of column vials mounted vertically spaced from each other, at least one nozzle in the column body is arranged and which extends away from the column body, and has a closable access opening, which is formed at the nozzle, wherein the column is characterized in that in a vertical section of the column directed into the column cavity line of the lower section line Stutzens or a tangent to this line of the lower line of intersection of the neck at least in sections, with the vertical inner line of the column body extending from the neck down, an angle in a range of 210 ° to 267 ° includes. In an advantageous embodiment, this angle is in a range of 225 ° to 267 ° and preferably in a range of 255 ° to 267 °.
  • the line of the lower cut line of the neck which is directed into the column cavity in the case of a vertical section of the column, is part of the surface of the neck. Further, the vertical inner line of the column body extending downwardly from the nozzle is a part of the inner surface of the column body.
  • top refers to the orientation of the column during operation.
  • dead zones in the column.
  • the residence time of the fluid in the column is particularly long.
  • Such a long residence time favors the polymerization.
  • dead zones can form in particular in the region of the inspection opening, in particular in the lower part of the nozzle.
  • the bottom wall of the nozzle extends horizontally away from the column body. On this horizontal surface, however, liquid can accumulate, which lingers longer in the column. If a polymerizable material is treated in the column, there is thus on this horizontal surface of the nozzle of the inspection opening to an unwanted polymerisation.
  • this polymerisation can be prevented by tilting the lower part of the neck so that liquid, which deposits on the surface of the neck pointing into the column cavity, runs back into the column cavity.
  • the angle of inclination should be at least 3 °, in which case the angle of the column cavity line is the bottom line of intersection of the neck with the vertical inside line of the column body extending downwardly from the neck 267 °.
  • the inclination is preferably even greater, too large inclinations lead to larger openings in the column body for the nozzle.
  • the choice of angle thus represents a compromise between a suitable inclination of the lower surface of the nozzle to the horizontal on the one hand and a suitable diameter of the nozzle on the other hand.
  • an angle in a range of 210 ° to 267 ° prefers an angle in a range of 225 ° to 267 °, and more preferably an angle in a range of 255 ° to 267 °.
  • sections, the inclination, ie the angle to the horizontal, the lower surface of the nozzle may also be lower, that is, the above-mentioned angle greater than the specified angle.
  • 70%, more preferably 90%, and in particular 100%, of the lower cutting line of the connecting piece fall into the aforementioned angular range.
  • the neck of the column has an upper half and a lower half.
  • the column cavity surface of the nozzle or the tangent to the surface of the nozzle with the vertical inner surface of the column body extending downwardly from the nozzle forms an angle in a range of 210 ° to 267 °, preferably an angle in a range of 225 ° to 267 °, and more preferably an angle in a range of 255 ° to 267 °.
  • the undesired polymer is formed especially at the surfaces of this lower half of the nozzle. Said choice of the angle to the vertical inner surface of the column body prevents liquid from remaining on the surfaces of the lower half of the nozzle and forming polymer.
  • connection piece is rotationally symmetrical about a horizontal axis.
  • the entire surface of the nozzle directed into the column cavity or the tangent on the surface of the nozzle with the vertical inner surface of the column body encloses an angle in the range of 210 ° to 267 °, preferably an angle in the range of 225 ° ° to 267 ° and most preferably an angle in a range of 255 ° to 267 °.
  • a horizontal axis rotationally symmetrical nozzles have opposite oblique nozzle, ie for example nozzles with parallel side surfaces which are mounted obliquely in the wall of the column body, the advantage that they are easier to install manufacturing technology. Further, the advantage of having the spout forming a hand hole is that this hand hole makes it easier to reach into the column cavity and see in it. This is not so easily possible, especially with oblique nozzles, if their axis is not aligned horizontally, ie not perpendicular to the column wall.
  • such nozzles have the advantage that the liquid runs from the inner wall of the column cavity above the nozzle to the inner wall of the nozzle, there continues to run down further to finally run off again from the inner wall of the column cavity below the nozzle. If the nozzle has an inner wall which is inclined upwards in this running direction, this process would be hindered and liquid would accumulate on one edge. There the liquid will drip off partly. However, there is a risk that liquid will accumulate at this edge. This is especially at oblique nozzle with parallel side surfaces of the danger. Namely, they have an inner surface which slopes upwards in the direction of travel.
  • the nozzle may be formed, for example, frustoconical.
  • the surface of the spigot directed into the column cavity then encloses an angle with the vertical inner surface of the column body which lies in the above-mentioned range.
  • liquid that deposits on the surface of the neck can drain particularly well back into the column cavity.
  • the nozzle is arranged in particular in the vertical direction between two trays mounted in the column cavity. These two floors do not necessarily have to be adjacent. There may also be other floors between these two floors in the area of the nozzle.
  • the inspection opening is a manhole opening, which is formed at the nozzle and which can be closed with a lid. If in this case at least one of the floors is mounted in the region of the manhole opening, a plate is advantageously arranged in the region of the connecting piece between the one floor and the closed cover.
  • this plate can be advantageously prevented that ascending gas or descending liquid flows past a horizontal opening in the region of the manhole opening at the bottom, which is mounted in the region of the manhole opening.
  • the entire cross-section of the column body in the region of the nozzle is substantially filled by the one bottom in the region of the manhole opening and the plate. Only at the joints may openings remain.
  • the plate is preferably designed as a mass transfer plate. In particular, this mass transfer plate also has openings through which gas can rise and liquid can descend, whereby a mass transfer is effected.
  • the one bottom in the region of the manhole opening and the plate are, in particular, aligned substantially horizontally.
  • the lid may be pivotally attached to the neck.
  • the plate may be attached to the lid so that it is removed when the lid is removed from the neck or swung away.
  • the inspection opening formed in the neck in particular has a circular cross-section. However, other round, oval or, more rarely, even rectangular cross sections are possible.
  • the clear width of the inspection opening is in a range of 100 mm to 800 mm. If the inspection opening is designed as a manhole opening, the clear width is in particular in a range of 400 mm to 800 mm. Only if it is planned to take large tools or other large parts with through the manhole opening, this opening can be made even larger. If the inspection opening is designed as a hand hole opening, the clear width is smaller, in particular in a range of 100 mm to 300 mm.
  • the soil used in the column according to the invention is in particular a dual-flow tray.
  • the risk of polymerization is when using a fluid mixture which
  • the trays which are mounted in the column can also be other trays, as described in the introduction. Between the floors further separation-effective internals can be arranged. Due to the separation-effective internals, the separation of substances in a column, which is used as a separation column, improved.
  • These further installations can be provided, for example, in the form of packages, in particular structured or ordered packages, and / or fillings.
  • packages those with rings, spirals, saddles, Raschig, Intss or Pall rings, Berl or Intalox saddles, Top-Pak etc. are preferred.
  • particularly suitable packages are z. B. packs of Julius Montz GmbH in D-40705 Hilden, such.
  • the pack Montz-Pak B1 -350 Preferably used perforated structured packages of stainless steel sheets. Packing columns with ordered packs are known in the art and z. In Chem.-Ing.Tech. 58 (1986) No. 1, pp. 19-31 as well as in the Technical Review Sulzer 2/1979, p. 49 et seq. Of the Brothers Sulzer Aktienge- Seilschaft in CH-Winterthur.
  • a spraying device is arranged in the column body, with which liquid can be sprayed at least against the surface of the nozzle, ie the inner surface of the nozzle, directed into the column cavity.
  • the spraying device it is also possible for the spraying device to be arranged in the column body, with which liquid can be sprayed at least against the inner surface of the nozzle, if in the region of the inspection Opening a floor is arranged. In this way, in each case the undesired formation of polymer is prevented.
  • the spraying device has a spray nozzle, a feed line and a spray liquid feed device.
  • the spray liquid has a spray nozzle, a feed line and a spray liquid feed device.
  • Feeding device is designed to remove spray liquid from the column cavity, to supply the extracted spray liquid via the feed line of the spray nozzle and to spray at least against the inner surface of the nozzle by means of the spray nozzle.
  • the spray liquid is removed above a base mounted in the column cavity and in particular not in the column sump.
  • the use of the liquid in the column cavity as the spray liquid affords the advantage that the spray liquid has substantially the same composition as the liquid washed away at the inner surface of the nozzle.
  • the spray liquid supply device has an inlet opening which is arranged directly above a bottom which is adjacent to the nozzle.
  • the inlet opening is arranged directly above the bottom, which is arranged directly below the nozzle.
  • the spray liquid is taken from the column cavity in an area which is adjacent to the height of the nozzle, in particular directly under the nozzle.
  • the column according to the invention can be used in particular as a separation column.
  • the separation column has a sequence of soils.
  • the clear distance between two directly successive trays within the column according to the invention is in particular not more than 700 mm, preferably not more than 600 mm or not more than 500 mm. In terms of application, the clear distance within the floor sequence is 300 to 500 mm. As a rule, the ground clearance should not be less than 250 mm.
  • the height of the column body is, for example, greater than 5 m, in particular greater than 10 m. However, it is also possible that the height of the column body exceeds 30 m or 40 m.
  • the invention further relates to a thermal separation process between at least one gas rising in a column as described above and at least one liquid descending in the column. In particular, the ascending gas and / or the descending liquid contains
  • the thermal separation process according to the invention may e.g. a fractional condensation process for separating acrylic acid from a product gas mixture containing acrylic acid of a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (in particular propene and / or propane) of the acrylic acid with molecular oxygen to acrylic acid.
  • a C3 precursor compound in particular propene and / or propane
  • the separation column (condensation column) can be designed as described in DE 10243625 A1 or WO 2008/090190 A1.
  • FIG. 1 shows a schematic view of a column according to an embodiment of the invention
  • FIG. 2 shows a detail view of a vertical cross section of the column shown in FIG. 1 in the region of an inspection opening
  • FIG. 3 shows a horizontal cross section of the column shown in FIG.
  • FIG. 4 shows a detailed view of a vertical cross section of a further embodiment of the column according to the invention
  • FIG. 5 shows a detailed view of a vertical cross section of yet another
  • the embodiment described below relates to a separation column 1, as z. B. in a process of fractional condensation for the separation of acrylic acid from an acrylic acid-containing product gas mixture of a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (in particular propene and / or propane) of acrylic acid is used with molecular oxygen to acrylic acid.
  • a C3 precursor compound in particular propene and / or propane
  • the known separation column 1 is shown schematically. It comprises a cylindrical column body 2 whose axis is vertically aligned.
  • the column body 2 is essentially a hollow cylinder. This means, the jacket 7 of the column body 2 forms a column cavity 3.
  • the column body 2 is made of stainless steel.
  • the separation column 1 is normally thermally isolated in a conventional manner.
  • the height of the separation column 1 is 40 m.
  • the inner diameter of the jacket 7 of the column body 2 is 7.4 m throughout.
  • the separation column 1 is subdivided into three regions: the upper region A is referred to as the column head.
  • the column head an inlet 4 is provided, via which a liquid can be introduced into the column cavity 3. Further, an exhaust pipe 13 is formed at the top for removing the gaseous mixture.
  • region B is formed below the column head a region B is formed. In this area, the fractional condensation is carried out. In region B, a removal line 14 is arranged, via which crude acrylic acid is removed.
  • region C Below the region B, the bottom of the column is formed in region C.
  • a feed line 5 for introducing the product gas mixture into the column cavity 3.
  • a drain 6 for the bottom liquid in the bottom of the column.
  • trays 8 are fixed in the column cavity 3.
  • the trays 8 of the column 1 are horizontally aligned and mounted vertically spaced from each other in the column cavity 3.
  • 8 downwardly oriented horizontal surfaces are formed in the soils.
  • the trays 8 serve as separating internals, which improve the material separation in the separation column 1.
  • the floors 8 are dual-flow floors. However, it is also possible to use other of the initially mentioned soils.
  • At least one inspection opening 9 is formed in the column body 2.
  • the jacket 7 or the column body 2 has an opening.
  • the cross section of the opening is circular. However, other cross-sectional shapes may be used as needed.
  • a frustoconical nozzle 1 1 attached.
  • the symmetry axis of the nozzle 1 1 is oriented horizontally, so that the nozzle 1 1 extends away from the column body 2.
  • the remote from the column body 2 end of the nozzle 1 1 forms the inspection opening 9.
  • a lid 12 is provided.
  • the lid 12 is pivotally attached to the nozzle 1 1. When closed, the lid 12 closes the inspection opening 9 liquid and gas tight.
  • the column cavity 3 via the access opening 9 is accessible from the outside.
  • the column body 2 comprises a plurality of spaced apart in the vertical direction nozzle 1 1 with the associated inspection openings.
  • the diameter of the inspection opening 9 depends on the purpose of the inspection opening 9.
  • the inspection opening 9 is formed as a manhole opening.
  • the diameter of this manhole opening is in a range of 400 mm to 800 mm.
  • FIG. 2 shows a vertical cross section of the column 1 shown.
  • the surface 15 of the lower section of the nozzle 1 1 which is shown in Figure 2 because of the sectional view as a line, closes with the vertical inner surface 16 of the column body 2, which extends from the nozzle 1 1 downwards and in FIG 2 is also shown as a line because of the sectional view, the angle ⁇ .
  • the angle ß is greater than 0, d. H. the surface 15 is not horizontally aligned at the lower line of intersection of the vertical cross section of the column 1, but inclined.
  • the angle of inclination is 3 ° in the present exemplary embodiment, with the drawings not rendering the angles true to reality for better illustration.
  • the angle ⁇ is thus 267 ° in this case.
  • the angle ⁇ can also be smaller, so that a greater inclination of the surface 15 results.
  • the angle ⁇ is in a range of 210 ° to 267 °, in particular in a range of 225 ° to 267 ° and preferably in a range of 255 ° to 267 °.
  • the inclination of at least 3 °, in particular in the lower region of the nozzle 1 1 is required so that liquid can drain.
  • the lower half of the neck 1 1 has this angle to the inner surface 16 of the column body 2.
  • the nozzle 1 1 is preferably rotationally symmetrical, so that the angle between the directed into the column cavity 3 surface of the nozzle 1 1 with the inner surface 16 of the column body 2 over the entire circumference of the nozzle 1 1 is the same.
  • the inner line which is part of the inner surface 15 of the nozzle 1 1, a straight line. In other embodiments, however, this line may also be bent.
  • the tangent to the surface 15 of the lower cutting line of the nozzle 11 with the vertical inner surface 16 of the column body 2 is considered.
  • a curved line changes the orientation of this tangent.
  • the above-mentioned angle ⁇ is in this case at least 50%, preferably over a larger range, such as. B. 70% or 90% in the specified angular range.
  • the angle ⁇ is in particular in no area 270 ° or larger.
  • a mass transfer tray 8-3 is also arranged in the area of the inspection opening 9. The distance between the two mass transfer trays 8-1 and 8-3 or between the two mass transfer trays 8-3 and 8-2 is then 500 mm.
  • the mass transfer tray 8-3 in the exemplary embodiment described is a dual-flow tray which has openings 17, as shown in FIG.
  • a plate 18 is arranged in the region of the inspection opening 9, which prevents gas rising in particular, but also descending liquid, from flowing upward past the mass transfer tray 8-3 through the horizontal opening formed by the nozzle 11 flowing down.
  • the plate 18 has openings 19 so that it acts as a mass transfer plate.
  • the plate 18 is oriented horizontally, being flush with the mass transfer tray 8-3.
  • the plate 18 is thus arranged horizontally at the same height as the mass transfer tray 8-3.
  • the shape of the plate 18 is as shown in Figure 3 to the horizontal cross-sectional shape of Adapted tail. Since the neck in the present embodiment is truncated cone-shaped, the plate 18 is trapezoidal.
  • the long side of the trapezoid of the plate 18 could also be adapted to the rounding of the mass transfer tray 8-3 in this area or vice versa the rounding the mass transfer tray 8-3 be flattened adapted in this area to the long side of the trapezoidal plate 18.
  • a plurality of plates 8 may also be located in the region of the inspection opening 9. These mass transfer trays 8 are then each assigned a plate 18.
  • the plate 18 is fixed to the pivotable cover 12 so that it is pivoted out with the lid 12 when the inspection opening 9 is opened. This has the advantage that the plate 18 does not have to be dismantled when inspection or cleaning work in the column 1 must be performed.
  • the mass transfer tray 8-3 is removable, so that a person can pass through the formed as a manhole access opening 9 in the column cavity 3.
  • the exemplary embodiment shown in FIG. 4 differs from the exemplary embodiment shown in FIGS. 1 to 3 in that no mass transfer tray 8-3 is arranged in the region of the inspection opening 9.
  • the inspection opening 9 is also not formed as a manhole, but as a hand hole.
  • the diameter of the inspection opening 9 is thus substantially smaller than in a manhole. It is designed so that the hand or the arm of a person together with z. B. a cleaning device in the column cavity 3 can be introduced.
  • the diameter is z. B. in a range of 100 mm to 300 mm.
  • the geometry of the nozzle 1 1 and in particular the inclination of the directed into the column cavity 3 surface 15 of the nozzle 1 1, in particular the lower section line of the nozzle 1 1 in a vertical cross-section of the column 1, is the same as in the embodiment of Figure 1 to 3.
  • a spray device 20 is arranged in the column body 2.
  • the spray device 20 is a liquid 22 at least against the directed into the column cavity 3 surface 15 of the nozzle 1 1 sprayable.
  • the spraying device 20 has a spray nozzle 21, which is supplied via a supply line 23 liquid.
  • the supply line 23 passes through a gas and liquid-tight passage 24 through the column body 2.
  • a pump 25 is arranged, which is connected to the supply line 23.
  • the pump 25 is connected to a line 26 which re-enters the column cavity via another gas and liquid-tight passage 27.
  • the conduit 26 has an inlet opening 28, which is arranged immediately above the mass transfer tray 8-1.
  • the mass transfer tray 8-1 is adjacent to the inspection opening 9 or the nozzle 11.
  • this mass transfer tray 8-1 immediately below the access opening 9.
  • liquid which has collected on the mass transfer tray 8-1, removed and from the spray nozzle 21 against the surface 15 of the nozzle 11 and the Inner surface of the lid 12 sprayed. This prevents liquid from accumulating and polymerizing in this area.
  • the nozzle 1 1 as in the previous embodiments is frustoconical.
  • the spraying device 20 can be used in other embodiments, however, at inspection openings 9 with smaller clear width and / or in columns 2, in which a bottom 8-3 is arranged in the region of the inspection opening 9.
  • the spraying device 20, starting from the supply line 23, may also comprise a line system which sprays the inner surfaces of further inspection openings with liquid.
  • the composition of the liquid withdrawn via the inlet opening 28 is not always substantially the same as the composition of the liquid in the region of the respective inspection opening 9 during operation of a separation process in which, in particular, gas rises and a liquid descends.
  • the process is a thermal separation process between at least one gas rising in the separation column 1 and at least one liquid descending in the separation column 1.
  • the ascending gas and / or the descending liquid contains (meth) acrylic monomers.
  • a fractionating condensation is carried out to separate acrylic acid from a product gas mixture containing acrylic acid a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (especially propene and / or propane) of the acrylic acid with molecular oxygen to acrylic acid in a separation column 1 containing separating internals.
  • the separation column contains from bottom to top first dual-flow trays and then cross-flow hood floors, which are supported from below as described above. Otherwise, the method is carried out as described in DE 19924532 A1, DE 10243625 A1 and WO 2008/090190 A1.
  • C3 precursor of acrylic acid is taken to mean those chemical compounds which are obtainable formally by reduction of acrylic acid.
  • Known C3 precursors of acrylic acid are e.g. Propane, propene and acrolein. But also compounds such as glycerol, propionaldehyde, propionic acid or 3-
  • Hydroxypropionic acid belongs to these C3 precursors. From them, the heterogeneously catalyzed gas phase partial oxidation with molecular oxygen is at least partially an oxidative dehydrogenation.
  • said C3 precursors of acrylic acid typically with inert gases such as e.g. molecular nitrogen, CO, CO 2, inert hydrocarbons and / or steam diluted, passed in admixture with molecular oxygen at elevated temperatures and optionally elevated pressure over transition metal mixed oxide catalysts and oxidatively converted into an acrylic acid-containing product gas mixture.
  • inert gases such as e.g. molecular nitrogen, CO, CO 2, inert hydrocarbons and / or steam diluted
  • the acrylic acid-containing product gas mixture typically comprises a heterogeneously catalyzed gas-phase partial oxidation of C3 precursors (eg propene) of acrylic acid with molecular oxygen over catalysts in the solid state, based on the total amount of the constituents (contained in it) Contents on:
  • inert gases e.g. Nitrogen, carbon monoxide, carbon dioxide, methane and / or propane.
  • the partial gas phase oxidation itself can be carried out as described in the prior art.
  • the partial gas phase oxidation may e.g. in two consecutive oxidation steps, e.g. in EP 700 714 A1 and in EP 700 893 A1.
  • the gas phase partial oxidations cited in DE 19740253 A1 and in DE 19740252 A1 can also be used.
  • the temperature of the product gas mixture leaving the partial gas phase oxidation is 150 to 350 ° C., frequently 200 to 300 ° C.
  • the hot product gas mixture is expediently first cooled to a temperature of 100 to 180 ° C, before it is conducted for the purpose of fractional condensation in the region C (the bottom) of the separation column 1.
  • the pressure prevailing in the separation column 1 operating pressure is usually 0.5 to 5 bar, often 0.5 to 3 bar and often 1 to 2 bar.

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  • Chemical Kinetics & Catalysis (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Devices For Use In Laboratory Experiments (AREA)

Abstract

La présente invention concerne une colonne (1) de traitement thermique de mélanges fluides comprenant un corps de colonne (2) cylindrique orienté verticalement qui forme une cavité de colonne (3) et une surface intérieure (16) verticale, plusieurs fonds (8) montés dans la cavité de colonne (3) et espacés entre eux verticalement, au moins une tubulure (11) qui se trouve dans le corps de colonne (2) et qui s'étend en s'éloignant du corps de colonne (2), et une ouverture de révision (9) qui peut être refermée et qui est formée au niveau de la tubulure (11). La colonne selon l'invention est caractérisée en ce que pour une section transversale verticale de la colonne (1) la surface (15) dirigée dans la cavité de colonne (3) de la ligne d'intersection inférieure de la tubulure (11) ou une tangente à la surface (15) de la ligne d'intersection inférieure de la tubulure (11) forme avec la surface intérieure verticale (16) du corps de colonne (2) qui s'étend vers le bas à partir de la tubulure (11), au moins par sections un angle allant de 210° à 267°.
EP16736065.0A 2015-07-17 2016-07-05 Colonne de traitement thermique de mélanges fluides, contenant notamment des monomères (méth)acryliques Withdrawn EP3325121A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US201562193609P 2015-07-17 2015-07-17
DE102015213490.3A DE102015213490A1 (de) 2015-07-17 2015-07-17 Kolonne zur thermischen Behandlung von fluiden Gemischen, insbesondere solchen, die (Meth)acrylmonomere enthalten
PCT/EP2016/065763 WO2017012853A1 (fr) 2015-07-17 2016-07-05 Colonne de traitement thermique de mélanges fluides, contenant notamment des monomères (méth)acryliques

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EP3325121A1 true EP3325121A1 (fr) 2018-05-30

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US (1) US20170014729A1 (fr)
EP (1) EP3325121A1 (fr)
CN (1) CN107847810A (fr)
BR (1) BR112018000792A2 (fr)
DE (1) DE102015213490A1 (fr)
WO (1) WO2017012853A1 (fr)

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CN107847810A (zh) 2018-03-27
WO2017012853A1 (fr) 2017-01-26
BR112018000792A2 (pt) 2018-09-04
US20170014729A1 (en) 2017-01-19

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