WO2005092464A1 - Trennboden für eine destillationskolonne - Google Patents
Trennboden für eine destillationskolonne Download PDFInfo
- Publication number
- WO2005092464A1 WO2005092464A1 PCT/EP2005/003271 EP2005003271W WO2005092464A1 WO 2005092464 A1 WO2005092464 A1 WO 2005092464A1 EP 2005003271 W EP2005003271 W EP 2005003271W WO 2005092464 A1 WO2005092464 A1 WO 2005092464A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- partition
- base plate
- substance
- attachment
- flow
- Prior art date
Links
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
- B01D3/16—Fractionating columns in which vapour bubbles through liquid
- B01D3/22—Fractionating columns in which vapour bubbles through liquid with horizontal sieve plates or grids; Construction of sieve plates or grids
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- 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
- B01D3/008—Liquid distribution
-
- 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
-
- 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
- B01D3/326—Tray supports
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- 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
Definitions
- the invention relates to a separating tray for a column for the distillation of a polymerizable substance, a process for producing a polymerizable substance and the use of a polymerizable substance obtainable according to the above process, and also chemical products based on the polymerizable substance as the starting compound.
- all of the monomers used in the radical polymer are suitable as polymerizable substances.
- Distillation columns are known for example from WO 00/53561. Although this document discloses the use of "dual-flow trays" as column trays with which the separation performance is to be increased, no measures are disclosed which are intended to counter the above disadvantages.
- the aim of this invention is in particular to extend the time interval between maintenance intervals of such distillation columns, preferably also reducing the downtimes significantly.
- Another object is to achieve the highest possible degree of purification in the course of the distillation process over a plurality of separating trays, with exactly reproducible or predetermined chemical processes taking place at each separation stage.
- a further object of the invention is to provide a homogeneous distribution of the polymerizable substance in the liquid or gaseous phase in a separation stage without the formation of polymer deposits.
- the separating tray according to the invention for a column for the distillation of a polymerizable substance comprises at least one tray plate with a multiplicity of openings and at least one attachment which divides the multiplicity of openings into groups, passages through which a fluid can flow through being formed with the at least one attachment.
- the base plate preferably comprises metallic material, however other temperature and acid resistant materials can also be used.
- the outer shape of the base plate is to be chosen with regard to the distillation column so that it can have, for example, round, rectangular or similar shapes.
- the base plate is provided with a multiplicity of openings, which means in particular that a liquid and / or gas exchange is possible through the base plate.
- the openings are preferably so large that the liquid substance can be backed up, preferably even a bubble layer for heat and component exchange is formed between the liquid and vaporous substances.
- the orientation of the openings with respect to the base plate can in principle be chosen freely and must be compared with the conditions inside the column.
- the attachment divide the plurality of openings into groups, with passages through which a fluid can flow through being formed with the at least one attachment.
- a primary function of this attachment is to influence the movement of the liquid that has accumulated on the base plate in such a way that on the one hand a high flow rate is avoided, but on the other hand no "dead zones" are formed in which the liquids have relatively long dwell times to rule.
- Particularly high flow rates can occur, for example, if the gaseous substance passing through the base plate is not introduced completely uniformly over the cross section of the base plate, but rather a particularly strong source is formed in one area. Then there may be a wave-like excitation of the liquid.
- the attachment serves as a kind of breakwater in that upper layers of the liquid or vapor bubble are vibrated.
- the spatially strictly separated division of the base plate into different sectors does not necessarily guarantee a better flow behavior of the liquid. Rather, the division may result in groups of openings which are less exposed to the polymerizable substance, so that the sectors may differ from one another. which result in different degrees of distillation. For this reason, it is proposed that the liquid be restricted in its freedom of movement by the attachment, but not limited in terms of the accessibility of a large number of openings in other sectors (in particular all openings). This is ensured by the fact that passages through which the fluid can flow are formed. The passages ensure that the fluid can preferably flow to any opening in the base plate.
- the shape of the passage is again to be chosen taking into account the liquid, the polymerizable substance, the column or its operation. Round passages, rectangular passages, slots, etc. may be mentioned here as examples. It should also be made clear that the passages can be completely or partially delimited or formed by the attachment. Basically, when arranging such passages, it is advantageous to place them in lower, i.e. Arrange areas near the floor slab. This ensures that, on the one hand, the propagation of the wave movement of the upper liquid or fluid layers is interrupted, while deeper layers near different groups of openings can communicate with one another. Care should be taken to ensure that the passages are designed in such a way that as few, preferably none, dead zones are formed, meaning zones in which the fluid has a relatively long residence time.
- the liquid tends to polymerize in such dead zones, which in the long term can lead to at least partial blockage of the openings.
- the consequence of this is that the gas or liquid exchange only takes place through a smaller number of openings, the increasing gas pressure resulting in additional vibration excitation of the liquid.
- the distillation step can no longer be carried out in the desired quality, which means that cleaning and maintenance measures are required. This in turn means that the distillation process has to be interrupted and the column has to be shut down.
- the partitions should be in a complex process cleaned and then assembled. Due to the attachment proposed here on the base plate, such complex measures can be postponed at least over a longer period of time.
- the passages extend from the base plate over a height in the range from 1 mm to 100 mm, preferably from 5 mm to 50 mm and particularly preferably from 10 mm to 30 mm.
- the openings are only partially limited by the attachment. In this case, they are at least partially limited by the base plate. It is possible that the passages are limited only by the base plate and the attachment, but other components can also be used to limit the passages.
- the height is selected so that the fluid can move or flow relatively unhindered in the vicinity of the base plate, and thus it is uniform. Flowing the openings with the liquid or the fluid is guaranteed. At the same time, the liquid layers away from the base plate are traversed by the attachment.
- the at least one attachment comprises at least one straight web.
- a design of the attachment is to be chosen in particular if the base plate also has straight edges, that is to say in particular is rectangular or square. This makes it possible in a simple manner to divide the openings in the base plate into groups of almost the same number. Under certain circumstances, however, it is also necessary that the attachment, in addition to straight webs or cut, curved guide surfaces, which cause such a flow of the impinging fluid that dead zones near the top are avoided.
- the orientation of the web in relation to the base plate can basically be chosen freely. This also means that the straight web extends over the entire base plate or even only partial areas of the base plate.
- the attachment has at least one of the following configurations: (a) a plurality of attachments with a web are provided; (b) an attachment with a plurality of webs, preferably connected to one another, is provided.
- the attachment can be constructed as a kit with a plurality of different or similar webs, but on the other hand, one-piece attachments or composite systems consisting of a plurality of webs, which are preferably connected by joining technology, are also suitable for production.
- the webs can be detachable or connected to one another by material bonding.
- the multiple attachments, each comprising a web are only in contact with one another via the base plate or other components of the column, while in the case of a one-piece, more complex attachments or the one attachment interconnected webs a direct connection or connection is formed via components of the webs or the essay itself.
- the configuration (b) has the advantage that it can be installed easily and with little expenditure of time. From these points of view, it may be advantageous that a complex attachment consisting of several webs is used in a central area, while in the peripheral areas, depending on the shape or shape of the attachment or the column, additional individual webs are used to complete the first attachment be positioned. It can thus be ensured that, for example, groups of openings with essentially the same number are formed.
- the at least one web has a length, the plurality of passages being at least partially limited by at least one of the following elements: (a) at least one strut which is part of the web; (b) at least one spacer which is a separate part; these elements having a width and the sum of the widths of the elements being less than 80%, preferably less than 60%, in particular less than 40%, of the length of the web.
- an easily assembled structural unit with the base plate is preferably proposed here. This means in particular that the bottom plate with the at least one attachment can be installed together in the column. As a result, the at least one attachment must be attached to the base plate itself. It is now proposed to do this via struts or spacers or both elements.
- the struts which are themselves part of the web, can be produced, for example, by shaping processes, such as casting, milling or the like. It follows that the struts are made of the same material as the web itself. Under certain circumstances, however, it is advantageous that the struts and the web itself are made of different materials, for example, the web is first produced in one piece and then the webs are connected to the web using a joining technique (detachable or non-detachable) ,
- separate spacers can be positioned on the base plate, which themselves comprise means for fixing the web.
- the webs can all be essentially rectangular, for example, the desired heights of the passages being able to be generated by different designs of the spacers. This results in cost-effective production of the webs on the one hand and a simple process-dependent adaptation of the passages.
- the struts or spacers are used in particular to stabilize or position the strut in relation to the base plate.
- the web is arranged, for example, in the edge regions of the base plate by means of a strut or a spacer on the base plate, while an additional element (strut or spacer) is provided in central regions depending on the length of the web.
- the sum of the widths of the struts or spacers is less than 80%, preferably less than 60% and particularly preferably less than 40% of the length of the web. It is therefore preferred that as few and preferably relatively slender elements are used to stabilize the web. This ensures that the flow of the fluid near the base plate can propagate relatively unhindered. In this case, it may be advantageous to equip the webs or spacers with a flow-wise favorable profile, in particular to form suitable flow-around edges (for example round cross-sectional shapes).
- the length of the web is the longest Describes expansion in one direction and the width of the strut or the spacer in the same direction is to be determined, wherein the width and the length can be arranged in one plane or in mutually parallel planes.
- the partition is designed such that the at least one attachment forms sectors of the base plate with a group of openings each, the sectors preferably having an area in the range from 1.2 m 2 to 0.3 m 2 , preferably 1 , 0 m 2 to 0.5 m 2 and in particular 0.8 m 2 to 0.6 m 2 .
- such dividers can be formed with a one-part or a multi-part base plate from several individual base plates, whereby it is basically ensured that an unevenness of the base plate of less than 3 mm / m, in particular mine 2 mm / m and preferably less than 1 mm / m is realized.
- a round base plate preferably has a total diameter in the range from 2 m to 7 m, in particular 3 m and 5 m.
- the openings in the base plate preferably have a diameter of 15 mm to 40 mm, in particular 20 mm to 30 mm.
- the partition plate have a cover plate, which is preferably arranged at a distance in the range from 60 mm to 200 mm, preferably from 80 mm to 150 mm and particularly preferably from 100 mm to 120 mm from the base plate and in particular also has a plurality of openings.
- the cover plate has a number of different functions. For example, one function is to be seen in this way preventing or at least significantly reducing the fact that the rising vaporous substance entrains parts of the liquid substance accumulated on the base plate.
- the separated liquid, which accumulates on the cover plate when the vaporous substance rises, is again distributed evenly and fed back to the base plate underneath.
- the cover plate has openings that are not parallel to the preferred flow direction of the vapor Fabric run, but at an angle to it, for example with an angle between 10 ° and 50 °. This enables more intensive contact of the fabric with the cover plate.
- the cover plate favors at least the material or heat exchange, which creates a further improvement in the separation performance.
- a uniform outflow of the vaporous substance away from the just penetrated partition to the next is made possible.
- the cover plate thus acts like a flow straightener, which ensures an even flow to the following partition. Accordingly, the cover plate can be designed exactly like such a flow straightener with a grid or honeycomb structure or a perforated plate similar to the base plate.
- the cover plate has a thickness of at least 50 mm, preferably at least 100 mm, in particular 150 mm, but particularly preferably not greater than 300 mm.
- this comprises a holder which has at least one solid support which is in contact with the side of the base plate facing away from the at least one attachment, preferably over at least one dimension in the range from 200 mm to 1000 mm, preferably from 350 mm to 800 mm and particularly preferably from 400 mm to 600 mm. It is also possible for the supports to be at least partially oriented substantially perpendicular to one another and, if appropriate, to be connected to one another by connecting elements, the supports being able to be provided with different dimensions in different directions.
- the holder mentioned can take on a number of functions, in particular at least one of the following two functions being in the foreground here: fixing the separating tray in relation to the column or further Ren dividing floors, or increasing the rigidity of the dividing floor. If this holder is used for fixation, these are preferably arranged such that they extend to the edge region of the dividing tray so that they can be connected to components of adjacent components (for example the column or other dividing trays).
- the function relating to increasing the rigidity of the dividing floor comes to the fore in particular when the dividing floor or all floor panels together cover an area of more than 10 m 2 , preferably more than 13 m 2 and particularly preferably more than 15 m 2 .
- brackets ensures that the base plate is still flat and that lowering of the base plate in relation to edge regions is avoided in central areas.
- Such unevenness in the base plate would result in boundary layers being formed near the base plate would have a reduced tendency to flow and thus have a tendency to polymerize. Since these bumps would be relatively large, a very large number of openings could be blocked by the polymerization deposits.
- a solid support is understood to mean, in particular, a support without cavities, that is to say spaces which are completely surrounded by the material of the support, in the interior of the support, with the exception of inclusions or cavities caused by production.
- the carriers are preferably also not designed such that stiff, but nevertheless cavity-forming profiles are provided.
- the supports are attached to the side of the base plate that faces away from the liquid level. Accordingly, they do not serve to directly influence the flow, but only if necessary as trailing edges or surfaces for fluid or liquid, which has passed through the openings of the base plate or which is condensed on the holder or the partition.
- the at least one support near the bottom plate has at least one recess with an extent, the sum of the extent at least in the range from 80% to 30%, preferably from 70% to 40% and particularly preferably from 60% to 55% of dimension 46 lies.
- the cutouts have, inter alia, the function of allowing the vaporous substance to flow through them and, if necessary, of displaying tear-off edges for liquid flows trickling down on the carrier. The larger the surface of such a carrier, the more the liquid that has passed through the openings can accumulate there. Thus, there would also be a risk here that boundary layers would be formed in which polymerization would occur quickly. For this reason, it is proposed here that edges are formed already after short flow paths, which prevent further flow along the carrier as a result of gravity.
- the carrier is T-shaped, the at least one recess being substantially perpendicular to the base plate lying carrier part is arranged.
- the T-shaped configuration offers the advantages that the upper, essentially parallel to the base plate, provides a contact surface to the base plate, which ensures an even and relatively large surface area. There are sufficient options for connection to the base plate.
- the base plate has no openings in the area of the system with the carrier.
- this carrier part lying essentially parallel to the base plate has the advantage that when the liquid flows down, the first tear-off edge is formed after a short distance, namely exactly where the upper carrier part ends.
- the carrier part, which is arranged essentially perpendicular to the base plate is positioned far enough from this edge that an accumulation of liquid as a result of the surface tension is avoided in the region where the upper and lower carrier parts meet.
- the gaseous, polymerizable substance condenses on the underside of the carrier part lying essentially parallel to the base plate and that there is nevertheless the possibility that this liquid flows down on the carrier part lying essentially perpendicular to the base plate.
- the arrangement of at least one recess is proposed here.
- the provision of such cutouts is advantageous because material can be saved in this way and thus the manufacturing costs, the component weight and also the manpower for installing such partitions can be significantly reduced.
- the recesses may also have to be designed according to the criteria of lightweight construction, as is already widely used.
- the aspects of lightweight construction can be further strengthened by a suitable choice of materials.
- the at least one T-shaped support is arranged parallel to the floor plate.
- arranged foot with a dimension in the range from 50 mm to 100 mm, preferably from 60 mm to 90 mm and particularly preferably from 70 mm to 80 mm, the at least one recess at a distance of less than 10 mm, in particular directly adjacent to the foot, is arranged and preferably has a width in the range from 40 mm to 120 mm, preferably from 60 mm to 100 mm and particularly preferably from 75 mm to 85 mm.
- T-shaped beam is essentially based on two interests. On the one hand, care should be taken to ensure that the wearer is sufficient. provides the desired stiffness of the separating tray, on the other hand it must be taken into account that the heat capacity of such a support may play an important role in the operation of the distillation column. This means that in the event of temperature fluctuations inside the column, excessively large temperature differences between the gas flowing past and the carrier must not occur, since this results in an increased risk of condensation or polymerization of the substance.
- the at least one carrier and the at least one attachment are arranged perpendicular to one another.
- Such a stiffening of the floor slab by means of such a framework system means that the above-mentioned areas regarding the dimension or the width of the T-shaped support can be made slimmer, preferably in the lower half or lower third of the specified value range ,
- the partition plate be at least partially provided with a coating that has an improved sliding property for liquids compared to steel.
- such a coating extends at least partially over one of the following components: the base plate, the holder, the attachment, the spacers.
- the coating can extend from the surface of the components over a few micrometers to a few millimeters (preferably 50 ⁇ m to 1000 ⁇ m, in particular 100 ⁇ m to 800 ⁇ m, preferably 200 ⁇ m to 400 ⁇ m).
- a polyfluorocarbon, preferably Teflon, polyaniline lacquers or coating with a metal ion-free surface (for example glass) or also mixtures of at least two of these types of coating are proposed as the coating.
- glass which consists of cooled melts of silicon dioxide (SiO 2 ), calcium oxide (CaO), sodium oxide (Na 2 O), optionally with larger amounts of boron trioxide (BO 3 ), aluminum oxide ( AI_ 2 ⁇ 3 ), lead oxide (PbO), magnesium oxide (MgO), barium oxide (BaO) or potassium oxide (K 2 O) was preferred.
- This technical glass preferably consists of at least 50% by weight, more preferably at least 65% by weight and most preferably at least 80% by weight of SiO 2 .
- the partition plate in principle, it is also possible to at least partially produce the partition plate from a non-metallic material, so that a separate coating of the type mentioned above is not required.
- plastic or a composite e.g. made of Teflon and plastic
- Teflon and plastic can also be used to produce at least one component or the entire partition.
- the provision of the floor plate made of Teflon or plastic is particularly advantageous.
- the container has a plurality of partitions and at least one spray system is provided, with which an underside of at least one part with the polymerization capable substance is sprayable.
- a spraying system effectively removes portions of the polymerizable substance adhering to the underside of the separating base, so that polymerization at these points can be avoided.
- the configuration in which the bottom separating tray of the column is positioned within the reach of such a spraying system is preferred. It is advantageous that the spraying system is supplied with liquid polymerizable substance from the collecting basin of the container and that this is sprayed evenly distributed onto the underside of the partition.
- the spray system preferably has a plurality of nozzles which form spray regions which are uniformly distributed over the cross section of the separating base.
- the spray system is very particularly preferably operated at high pressure, for example in the range from 2 to 5 bar, preferably around 3 bar. It is further preferred that the spraying system is positioned at a short distance from the underside of the partition, for example at most 1 meter or 50 cm, whereby this can be varied taking into account the spraying area and / or the number of nozzles.
- the spray system described above should preferably be used in combination with a separating tray of the type described here according to the invention. Further details can be found in the description of the figures.
- the invention further relates to a process for purifying a polymer capable of polymerization, the polymerizable substance being introduced as a substance liquid in a column according to the invention through the feed and being converted into an at least partial substance gas phase in the interior.
- the substance-gas phase flows over a first partition plate arranged above the inlet with an isotropic density, the maximum deviation of an average value of the isotropic density being at most 15% within a plane between the inlet and the first partition plate. It is particularly advantageous if the maximum deviation is at most 10%, in particular only 5%.
- the plane is preferably relatively close and parallel to the first separating tray in order to ensure a relatively compact structure of the column.
- the plane is preferably at most 100 mm below the first partition, the distance of the plane from the first partition can also be a maximum of 50 mm or even a maximum of 10 mm.
- a particularly uniform distillation with a very low tendency to polymerize in the column is provided if the at least one separating plate is designed in such a way that the isotropic density is also established in the liquid phase of the polymerizable substance. This can be achieved to a particular degree by using a so-called "dual-flow tray". In this case, flows of the substance-gas phase over the dividing trays can be realized with the proposed isotropic density, the maximum deviation occurring further is significantly reduced.
- polymerizable substances are monomers used in the production of bulk plastics, such as styrene, methylstyrene, methyl methacrylate, butyl acrylate and the like. It is further preferred that the polymerizable substance used in the process according to the invention is (meth) acrylic acid.
- (meth) acrylic acid in the present case stands both for the compound with the nomenclature name “acrylic acid” and for the compound with the nomenclature name “methacrylic acid”, acrylic acid being preferred by both.
- the liquid substance is overheated.
- the temperature of the main component of the substance liquid is at least 1 ° C., preferably at least 5 ° C. is particularly preferably at least 10 ° C above the boiling temperature of the pure main component of the liquid substance.
- the invention relates to a method for producing a polymerizable substance, the polymerizable substance being synthesized from at least one product in a reactor and subsequently being subjected to a method according to the invention for purification.
- the synthesis of the polymerizable substance is not limited to a specific process. Rather, all methods known to the person skilled in the art can be considered.
- In the synthesis of acrylic acid there is a preferably at least two-stage gas phase oxidation reaction, in which acrolein is preferably obtained in a first step by catalytic oxidation of propylene and acrylic acid as a gas phase in a further step.
- This gas phase is then brought into contact in a quench unit with a liquid, preferably water or an organic compound boiling higher than water, or a mixture thereof, and is subjected directly or indirectly to the purification process according to the invention.
- a liquid preferably water or an organic compound boiling higher than water, or a mixture thereof.
- the invention relates to the use of an inlet according to the invention for the distillation of a polymerizable substance.
- the invention further relates to a polymerizable substance obtainable by a process according to the invention, the polymerizable substance preferably being acrylic acid or methacrylic acid, very particularly preferably acrylic acid.
- the invention relates to the use of a polymerizable substance according to the invention, preferably acrylic acid, as the starting compound in
- Molding compounds, fibers, foils, absorbent polymers in polymers for leather and textile processing, in polymers for water treatment or in polymers for soap production.
- the invention also relates to molding compositions, fibers, films, absorbent polymers, polymers for leather and textile processing, polymers for water treatment or in polymers for soap production, based at least in part on a polymer-capable substance according to the invention, preferably based on acrylic acid.
- Figure 1 shows schematically and in perspective the structure of a column with an inlet for a polymerizable substance.
- FIG. 2 schematically shows a sectional view through an embodiment of a partition
- FIG. 3 shows a schematic view of a further embodiment of a partition
- 4 shows a further schematic view of a further embodiment of the partition in section;
- 5 shows simplified, schematic representations of different embodiments of a flow straightener;
- 6 shows a schematic detailed view of an embodiment of a coated base plate of a separating base;
- FIG. 9 shows schematically and in perspective a corrugated base plate of a partition
- FIG. 11 shows a partial section of a container with a spray system in cross section
- Fig. 12 is a plan view of the spray system shown in Fig. 11.
- Fig. 1 shows schematically and in a sectional view a column 1 for distillation of a polymerizable substance, which comprises a container 2 with a bottom plate 8 and an inlet 4 for the polymerizable substance.
- the inlet 4 leads into an inner region 5 of the container 2.
- the column 1 has various means for uniformly distributing the substance in the container 2.
- the polymerizable substance is initially in the form of a liquid and is transformed or superheated into a vaporous or gaseous state by means of a heater 27.
- the substance flows in the direction of flow 25 through an inlet 4 into the inner region 5 of the container 2.
- the partly liquid, partly vaporous substance continues to flow in the direction of flow 25 ( here shown upright with the arrows) towards a separating plate 23 in which a first distillation stage is realized.
- Condensed constituents of the substance in the form of drops 26 fall again in the flow direction 25 in the opposite direction onto the inlet 4 or the underbody 8 of the container 2.
- the container 2 has a collecting basin 24, in which the condensate collects. This collecting basin is connected to a pump 28, which carries out the removal of the condensate in the collecting basin 24 from the column 1.
- the inlet 4 Upon closer inspection of the inlet 4, it can first be seen that it has an inlet opening 13 and an outlet opening 14, the outlet opening 14 being arranged closer and essentially parallel to the underbody 8 of the container 2.
- the inlet 4 is shown as a separate component which projects through a connection 3 through the container 2 into the inner region 5.
- the inlet 4 has straight and curved portions, these being designed so that the outlet opening 14 is aligned with its central axis 19 centrally to the central axis 62 of the container 2.
- a flow influencer 15 is arranged inside the inlet 4 over a distance 18 up to the outlet opening 14.
- the flow influencer 15 comprises a plurality of baffles 16 which ensure channels 17 for equalizing the flow of the polymerizable substance in the interior of the inlet 4.
- a cone-shaped flow is centered on the central axis 19 or the central axis 62.
- mung distributor 20 arranged so that its tip 21 is the outlet opening 14 closest.
- the arrangement of the flow distributor 20 in the inner region 5 of the container 2 results in a deflection of the inflowing substance, the container 8 additionally being designed so that it supports it the guide surfaces 61 support the uniform distribution of the substance in the container 2.
- the arrangement of the flow distributor 20 shown has the advantage that the inflowing substance is not directly mixed with the condensate stored in the collecting basin 24, so that the flow distributor 20 even has a protective function here.
- the inlet 4 is provided with a plurality of means for thermal insulation with respect to the inner region 5, these being arranged in a partial region 9 which extends the entire outer surface 6 of the inlet 4, which extends with the Inner area 5 of the container 2 is in contact.
- the inlet 4 is designed as a double-walled tube, so that it has two envelopes 10 which are arranged coaxially to one another.
- a thermally insulated layer 11 is embodied as a vacuum between the two envelopes 10, the inner surface 12 of the envelope 10 being mirrored.
- the entire outer surface 6 of the inlet 4 the entire lateral surface or tip 21 of the flow distributor 20 and also the inner wall of the Container 2 is provided with a coating 22 which has a sliding property for liquids which is improved compared to steel.
- FIG. 2 shows schematically and in a partial section a partition 23 which comprises a cover plate 41, an attachment 31, a base plate 29 and a carrier 44.
- the liquid 60 is arranged between the cover plate 41 and the base plate 29.
- the gaseous, po- lymerizable substance in flow direction 25 in contact with liquid 60; different boundary layers form between the base plate 29 and the cover plate 41.
- a liquid layer 56 can be seen which is essentially free of bubbles 59.
- a vapor bubble layer 57 or a kind of foam layer is arranged above it. This practically represents a kind of boundary layer between the liquid 60 and the gaseous volume.
- a drop layer 58 which is essentially characterized by a gaseous state of the substance to be distilled, that of liquid drops 26 starting from the cover plate 41.
- the gaseous substance moves in the direction of flow 25 (as shown in the figure) from the bottom up, the liquid 60 follows the gravitation 55 and falls in the opposite direction (countercurrent principle) towards the underbody 8 (not shown).
- the cover plate 41 cannot necessarily be constructed in one part but also in several parts.
- the cover plate 41 preferably comprises a plurality of structured sheets and / or plastic elements which are stacked into packs and form flow passages (preferably non-linear) between them.
- the sheets or plastic elements are preferably arranged essentially parallel to the direction of gravity, in particular at a distance 42 from the base plate 29 in the range from 100 to 200 mm.
- the sheets or plastic elements are advantageously provided in such a way that the cover plate 41 or the packing has a thickness of approximately 100 to 200 mm.
- the base plate 29 has a multiplicity of openings 30 which are divided into a plurality of groups 32 with the aid of the attachment 31 (see FIG. 3).
- the attachment 31 is nevertheless designed such that passages 33 through which the fluid or liquid 60 can flow are formed, which in the direction of the arrow 54 (ie essentially parallel to the base plate 29 or essentially perpendicular to the flow) direction 25 of the substance) ensures a liquid exchange from openings 30 arranged adjacent to one another.
- the attachment 31 is here provided with a coating 22 which has an improved sliding property for liquids compared to steel. At the same time, the attachment 31 acts as a spacer or support wall with respect to the two plates 29 and 41.
- the cover plate 41 is arranged at a predetermined distance 42 from the base plate 29, preferably parallel to the base plate 29. Taking into account the size or height 34 of the passages 33, it can be seen that the passages 33 are essentially somewhat smaller than the liquid layer 56, so that flow areas are obstructed in regions of the liquid layer 56 located above and close to the vapor bubble layer 57 , while relatively unimpeded liquid movements are made possible in the vicinity of the base plate 29 in the direction of the arrow 54.
- the cover plate 41 can also be designed as a flow straightener 64, in particular as a honeycomb structure 68 with a plurality of channels through which a fluid can flow.
- a carrier 44 is provided as a holder on the side 45 facing away from the paragraph 31.
- the carrier 44 is T-shaped and has a foot 49, which is arranged essentially parallel to the base plate 29 and has a predeterminable dimension 50, and a lower carrier part which is essentially perpendicular thereto.
- Recesses 47 are provided in the support part of the T-shaped support 44, which is essentially real to the base plate 29.
- the cutouts 47 are arranged at a distance 51 of less than 3 mm.
- a large number of tear-off edges 63 are formed, which have the consequence that flowing fluid (shown as a dash-dot line) forms drops 26 and detaches from the surface in the direction of gravity 55.
- both the base plate 29 and the carrier 44 are provided with a coating 22, which in particular comprises Teflon.
- FIG. 3 shows schematically and in a top view a further embodiment of a partition 23 according to the invention.
- the separating tray 23 shown spans the entire inner region 5 of the column 1 or the container 2. However, it is also possible for a plurality of such, then preferably rectangular, separating trays 23 to be combined to form a uniform platform which ultimately covers the entire inner region 5 of the column 1 spanned.
- the round embodiment of the partition 23 shown here has a plurality of openings 30, these being divided into a plurality of groups 32 by the attachment 31.
- the attachment 31 comprises a plurality of webs 35 which are connected to one another in a regular arrangement by means of joining technology.
- the attachment designed in this way forms sectors 40 of the base plate 29, each with a group 32 of openings 30.
- the attachment 31 is designed such that an exchange of liquid or fluid from adjacent sectors 40 is nevertheless ensured in the direction of the arrows 54.
- the carriers 44 are also shown in dashed lines on the lower side 45 of the base plate 29 provided with a coating 22. These are connected directly to the column 1 and serve, among other things, to increase the stability of the base plate 29.
- FIG. 4 shows a further sectional view for explaining an embodiment variant of the dividing plate 23 according to the invention.
- the holder 43 of the dividing plate 23 is realized with a carrier 44 which, via projections 53, connects with the container 2 of the column 1 is connected, so that an essentially horizontal positioning of the dividing plate 23 in the inner region 5 of the column 1 is ensured.
- the projections 53 are shown here in simplified form. In fact, a plurality of adjustment options can be provided, which enable the partition 23 in the interior 5 to be aligned exactly, horizontally.
- the carrier 44 shown has a dimension 46 and is T-shaped.
- the support 44 has a foot 49 which serves to support the base plate 29.
- a plurality of cutouts 47 adjoins this foot 49 directly in the vertical support part, these being formed here in a semi-ice-like manner.
- the semicircular design 47 is not mandatory, but has advantages in terms of rigidity due to its rounded contours.
- These recesses 47 can be described by an extent 48 which is to be determined essentially parallel to the base plate 29 or the foot 49.
- the recesses 47 each have a width 52 perpendicular to this.
- the cutouts 47 are preferably designed such that the sum of the expansions 48 is at least in the range from 80% to 30%, preferably from 70% to 40% and particularly preferably from 60% to 65% of the dimension 46.
- FIG. 4 An attachment 31 in the form of a web 35 is shown in FIG. 4 above the base plate 29.
- the web 35 is fixed by means of spacers 38 in the edge region of the base plate 29 near the container 2.
- spacers 38 alone would already create a gap between the web 35 and the base plate 29, which under certain circumstances would already result in the advantageous influencing of the fluid flow described here, hi Fig. 4 is now a special embodiment for illustration purposes of the web 35 is shown with individual webs 37.
- the webs 37 and the spacers 38 have a width 39, the sum of the widths 39 being significantly smaller than the length 36 of the web 35 (for example less than 50%).
- FIG. 5 shows schematic different embodiments of flow straighteners 64 which are used to improve the flow of the vaporous polymerizable substance to a separating plate 23. Basically, it should first be pointed out that such a flow straightener 64 fulfills the function of a uniform flow of the substance capable of polymerization to implement the at least one partition 23.
- uniform means that preferably at least one of the factors flow velocity and flow direction across the cross section of the inner region of the column 1 near the dividing plate 23 is only a deviation in the range of less than 20%, in particular less than 10% and advantageously less than 5% ,
- a symmetrical arrangement of the tolerance range with respect to the vertical flow direction is assumed.
- the flow straightener 64 is preferably of flat design and is aligned essentially parallel to the at least one separating plate 23 or is fixed in the inner region 5 of the column 1.
- the flow straightener 64 is preferably at least partially made of a corrosion and high temperature resistant material and can be flowed through by a fluid.
- openings are provided which on the one hand influence a flow profile, preferably with regard to speed and / or direction, but on the other hand prevent the openings from being blocked or closed.
- the flow straightener 64 preferably extends over the entire inner region 5 of the column 1.
- This flow straightener 64 accordingly comprises at least one of the following elements: at least one lattice structure 67, at least one honeycomb structure 68, at least one perforated plate 69 or a so-called packing. These elements can be connected directly or indirectly to the partition 23, in particular in particular a part of the partition 23.
- the lattice structure 67 comprises several elongated, fiber-like structures which are connected to one another chaotically or like a fabric. Coated metal wires, for example, are suitable as such elongated, fibrous structures.
- the honeycomb structure 68 can be made in one piece or from a plurality of components.
- the embodiment shown here comprises several smooth and structured sheet metal layers which are connected to form a honeycomb structure 68.
- the perforated plate 69 can also be rectangular, oval, polygonal or in some other way.
- the proportion of the holes is preferably more than 30% of the total area of the perforated plate 69.
- FIG. 6 shows a detail of an embodiment of a partition 23 comprising a base plate 29 with a coating 22 which has a lower adhesive property for liquids than steel. From the illustration it can be seen that the coating 22 can be described on the basis of the characteristic values layer thickness 71, surface roughness 72 and porosity 73.
- the coating 22, which preferably comprises polytetrafluoroethylene, is applied to contact surfaces 70 which would otherwise be in direct contact with the polymerizable substance. This prevents the substance from attaching and polymerizing.
- FIG. 7 schematically shows a plant for the production of acrylic acid which has a first gas phase oxidation reactor 76 for the oxidation of propylene to acrolein, which is connected to a further gas phase oxidation reactor 77 in which the acrolein is subjected to a further oxidation to acrylic acid.
- the acrylic acid gas mixture thus obtained in the further reactor 77 is fed to a quenching device 78, to which a column 1 according to the invention is directly or indirectly connected.
- One or more further cleaning units 79 can be connected to the column according to the invention.
- These preferably include crystallization devices such as layer crystallizers, suspension crystallizers, which are connected to washing columns, or extractors or aze- otropdestillatoren.
- the cleaning unit 79 is preferably arranged on the part of the column 1 where the acrylic acid is obtained in the greatest purity, which is preferably the column head 80.
- This design of the device for the production of acrylic acid gives it a very high purity, usually over 99.8%. Comparable device designs are also conceivable for the other polymerizable substances other than acrylic acid.
- FIG. 8 schematically shows the structure of a test arrangement for determining the density distribution of the substance-gas phase.
- the container 2 and the first partition 23 are shown in dashed lines.
- a line 85 below the partition 23 shows an imaginary plane 81 in which the isotropic density distribution in the substance-gas phase is determined.
- the level 81 is free of other components of the container 2 or of components arranged therein.
- a source 82 for radioactive radiation and a corresponding detector 83 for determining the amount of the incident radioactive radiation are provided on opposite areas of level 81.
- the source 82 sends a beam through the center 87 of the plane 81, which essentially corresponds to the cross section of the container 2.
- a further position of the source and the detector is also shown in dashed lines and identified by (II). Positions (I) and (II) were taken consecutively in time and with a change in direction 86 with respect to one another, a measuring process being carried out in each case.
- the detector 83 has counted the imping
- the measurement result is shown schematically in FIG. 8 using two bar-like graphs.
- the measurement was carried out over a predetermined period of time and with a certain beam width 88.
- the detector 83 each generated a graph which represents the distribution of the counting pulses (n) over the beam width 88.
- the maximum value of the first measurement (position I) and the second measurement (position II) are marked in the diagram with and nn.
- the integral of the counting pulses (n) over the beam width 88 is identified by Ai or An.
- the value or the shape of the respective integral or the value of the counting pulses is characteristic of the density of the irradiated medium or the irradiated substance gas phase.
- a bar-shaped configuration of the integrals or a high value of the counting pulses shows that a very large proportion of the radiation emitted by the source 82 has reached the detector 83. Conversely, a very low value of the counting impulses or a pointed form of the graph indicates a denser medium which is at least partially not penetrated by the radioactive radiation.
- a maximum deviation of the isotropic density within the plane 81 between the inlet 4 and the first partition 23 is at most 15% be.
- FIG. 9 schematically shows a detail of a special embodiment of a corrugated base plate 29 of a partition 23.
- a base plate 29 in particular with the following properties, has a large number of holes 30 and, in combination with the embodiment variants described here, is also special independently of it advantageous.
- the advantage of a corrugated base plate 29 is that the adhering liquid drops 26 run down to the corrugation troughs 90 and mix locally with one another there. This further reduces the risk of polymerization. At the same time, this accumulation of liquid ultimately causes it to detach.
- dividing plates 23 of a column 1 are equipped with such corrugated plate plates 29.
- Bottom plates 29 positioned adjacent to one another are preferably offset with respect to the alignment or orientation of the waveform, in particular in such a way that the crests 89 or troughs 90 of the bottom plates 29 form an angle of approximately 90 °.
- wave height 92 means the mean vertical distance between wave crest 89 and wave trough 90.
- a wave crest 89 is at a horizontal distance from its neighboring wave trough 90 (corresponds to the wave length 91) of approximately 3.0 cm to 10 cm, in particular the wave length 91 is in a range from 4.0 cm to 6.0 cm ,
- a further improvement with regard to the reduction in the tendency to polymerize can be achieved by special configurations of the areas of the column 1 which come into contact with the polymerizable substance. This applies in particular to at least part of the partition 23, the flow distributor 20, the inlet 4, the flow straightener 64 or the container 2.
- the mean roughness value is the arithmetic mean value (via a reference path 95) of the absolute amounts of the sections 96 of the actual profile 94 from the central position 93.
- the mean roughness value is preferably in a range of less than 2.0 ⁇ m (micrometers), in particular in a range of 0.5 ⁇ m to 1.0 ⁇ m. With such an average roughness value, the tendency of the liquid to adhere to the surface wetted by it is reduced, so that it runs faster or drains. 9 shows such an average roughness value with reference to the surface of the base plate 29 by way of example and illustration.
- This self-cleaning surface preferably has an artificial, at least partially hydrophobic surface structure of elevations and depressions, the elevations and depressions being formed by particles fixed on the surface by means of a carrier. It is advantageously characterized in that the particles have a fissured structure with elevations and / or depressions in the nanometer range (nanostructure 97 is shown schematically in FIG. 9).
- the elevations preferably have an average height of 20 to 500 ran (nanometers), particularly preferably 50 to 200 nm.
- the distance between the elevations or depressions on the particles is preferably less than 500 nm, very particularly preferably less than 200 nm.
- the fissured structures with elevations and / or depressions in the nanometer range can, for example, over cavities, pores, grooves, tips and / or peaks are formed.
- the particles themselves have an average size of less than 50 ⁇ m (micrometers), preferably less than 30 ⁇ m and very particularly preferably less than 20 ⁇ m.
- the particles preferably have a BET surface area of 50 to 600 m / g (square meters per gram).
- the particles very particularly preferably have a BET surface area of 50 to 200 m / g. With the so-called "BET surface", the well-known method of BRUNAUER, EMMET and TELLER is used to determine the specific surface.
- a wide variety of compounds from many areas of chemistry can be used as structure-forming particles.
- inorganic particles are preferred.
- the particles preferably have at least one material selected from silicates, doped silicates, minerals, metal oxides, silicas, polymers and metal powders coated with silicic acid.
- the particles preferably have pyrogenic silicas or precipitated silicas, in particular aerosils, Al 2 O 3 , SiO 2 , TiO 2 , ZrO 2 , zinc powder coated with Aerosil R974, preferably with a particle size of 1 ⁇ m (Mil ⁇ ometer) or powdery polymers such as cryogenic, ground or spray-dried polytetrafluoroethylene (PTFE) or perfluorinated copolymers or copolymers with tetrafluoroethylene.
- PTFE polytetrafluoroethylene
- Such particles or coatings for generating self-cleaning surfaces can be obtained, for example, from DEGUSSA AG.
- the isotropic density ("direction-independent" density distribution) of the gas phase or the deviation is determined, for example, using a method from Ingenieur remember Bulander & Esper GmbH in Zwingenberg, Germany.
- a directed beam (with a predetermined width, for example 5 cm) to a detector, the source and detector being located on opposite sides of the column, so that the beam extends essentially horizontally through the column, for example cobalt (Co 60) and Cesium (Cs 137) with an activity of 0.3 to 3.7 GBq is used.
- the beam emitted during the operation of the column is advantageously measured with a scintillation detector in the form of pulses per unit of time and passed on to an evaluation or display device.
- a scintillation detector in the form of pulses per unit of time and passed on to an evaluation or display device.
- a plurality of detectors or sources can also be provided, which are optionally distributed over the circumference of the column.
- the latter arrangement has the advantage that the same experimental setup can be maintained for comparison measurements in different directions and only other sources or detectors are used, so that measurement inaccuracies due to improper mounting can be avoided.
- a counter of the detector detects the incident radiation and counts the pulses.
- the number of pulses per unit of time is a measure of the density of the material between the source and the detector. A high value characterizes a low density because a large proportion of the emitted radiation has reached the detector. Accordingly, a low value of the counted pulses is characteristic of a higher density.
- a uniform flow of the substance-gas phase can be recognized, for example, by the fact that the liquid and gaseous components are evenly distributed in a cross section. This shows that the partitions are locally blocked (so that there is only a small amount of liquid in the substance-gas phase and thus a lower density) or, for example, areas of low gas flows (where then due to the lower counterpressure there is an increased liquid flow and thus an increased density can be determined).
- a characteristic value or a characteristic integral for the detected radiation has been recorded, the procedure described above is now repeated on the same level but in a different direction.
- the two directions enclose an angle that is preferably greater than 30 °, in particular even greater than 40 °.
- at least 2 such measurements are to be carried out from different directions, in particular even at least 3.
- a direction along the diameter of the column should be selected to ensure that the free beam length through the substance-gas phase is of the same length and thus the values for compare the detected radiation with each other. This is possible because the radiation has passed through the same volume of the substance gas phase.
- the level can in principle be arranged arbitrarily in the column and is preferably to be aligned essentially parallel to at least one separating plate. To check the uniformity of the flow, such directional radiation can be carried out through a separating plate, the distillate or through the substance gas phase. To characterize the flow behavior of the first partition, the level should preferably be selected in a range less than 200 mm below the first partition. In particular, the plane lies in a range from 100 mm to 10 mm below the first partition.
- An isotropy of the density in the sense of the invention is present in particular when the deviation of the measured values (n or N) recorded is at most 15%.
- An arithmetic mean (M) of the measured values is determined to determine the deviation.
- M arithmetic mean
- a maximum deviation of, for example, 5% means that the highest measured value of the pulse rate and the lowest measured value lie in a range from 0.95 M to 1.05 M.
- the measurement deviation due to cosmic ambient radiation approximately +/- 50 counting pulses with a measurement duration of usually 3 seconds and a measuring tape of approximately 50 mm
- the measurement deviation due to cosmic ambient radiation is preferably taken into account.
- FIG. 10 shows schematically and in perspective a further embodiment of the inlet 4 with a flow mixer 98 as a special embodiment of a flow influencer.
- the inlet 4 shown has a curvature 99 in which the polymerizable substance is deflected. If the polymerizable substance would flow freely through such an inlet 4 without a flow influencer, the curvature 99 would result in an uneven velocity distribution of the flow over the cross section of the inlet 4. The reason for this is flow eddies and backflows in the region of the curvature 99. In order to avoid this it is also possible to provide a flow mixer 98 upstream in the vicinity (preferably immediately before) the bend 99.
- Such a flow mixer 98 divides the inflowing polymerizable substance into a plurality of flow threads 100 and deflects them so that they cover essentially the same distance through the curvature 99.
- the polymerizable substance is preferably at least partially rotated.
- a uniform flow can thus be generated without pulsations and backmixing, so that the cross-section of the inlet 4 is evenly aerated even after the curvature 99 and the polymerizable substance hits the flow distributor 20 evenly distributed, for example.
- the provision of such a flow influencer or flow mixer 98 can take place at several bends 99 of the inlet 4.
- FIG. 11 illustrates a partial section of a container 2 with a spray system 101 in cross-section, wherein in FIG. 12 a top view of the parts shown in FIG. showed spray system 101 is shown.
- the container 2 is designed with a separating plate 23, the underside 105 (in particular during the operation of the column 1) is cleaned with a spray system 101.
- a spraying system 101 is preferably provided at least for the lowermost partition 23 of the container 2 if it has a plurality of partitions 23 arranged one above the other. A liquid of the polymerizable substance with a certain composition flows through this partition 23, which is then collected, for example, in a collecting basin 24 of the container 2.
- this liquid available to the spray system 101 via a delivery device 104 and thus to clean the underside of the separating base 23.
- the use of this liquid has the advantage that there is no significant influence on the distillation in the bottom separating tray 23.
- adhering (possibly already partially polymerized) constituents of the polymerizable substance are effectively removed from the underside 105 of the partition 23.
- the spray system 101 itself can be designed with a plurality of nozzles 102. These are designed such that the partition 23 can be cleaned substantially uniformly over its entire cross section. The arrangement and / or the type of nozzles can be selected accordingly.
- FIG. 12 schematically shows a possible embodiment of the spray system 101 with uniformly distributed nozzles 102 which have a spray region 103 which is essentially of the same type. Such a configuration of the spray system 101 is technically and economically simple, but is not absolutely necessary.
- the nozzles 102 are arranged here in such a way that the spray areas 103 do not essentially overlap, but this is also not mandatory. Both simple openings in the spraying system 101 and separate nozzle components (preferred) come into consideration as nozzles 102. LIST OF REFERENCE NUMBERS
- Liquid level first gas phase oxidation reactor further gas phase oxidation reactor
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007505482A JP2007530273A (ja) | 2004-03-29 | 2005-03-29 | 蒸留塔の分離フロア |
CN2005800173692A CN1960789B (zh) | 2004-03-29 | 2005-03-29 | 用于蒸馏塔的分离底盘 |
BRPI0509474-7A BRPI0509474A (pt) | 2004-03-29 | 2005-03-29 | partição de separação para uma coluna para destilação de material polimerizável, processos para a purificação e a produção de material polimerizável, material polimerizável, seu uso e produtos baseados no mesmo |
US11/547,109 US20070262022A1 (en) | 2004-03-29 | 2005-03-29 | Separating Tray for a Distillation Column |
EP05735782.4A EP1735068B1 (de) | 2004-03-29 | 2005-03-29 | Verfahren zur destillation eines polymerisationsfaehigen stoffes |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE102004015714A DE102004015714B3 (de) | 2004-03-29 | 2004-03-29 | Trennboden für eine Destillationskolonne |
DE102004015714.6 | 2004-03-29 |
Publications (1)
Publication Number | Publication Date |
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WO2005092464A1 true WO2005092464A1 (de) | 2005-10-06 |
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Application Number | Title | Priority Date | Filing Date |
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PCT/EP2005/003271 WO2005092464A1 (de) | 2004-03-29 | 2005-03-29 | Trennboden für eine destillationskolonne |
Country Status (8)
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US (1) | US20070262022A1 (de) |
EP (1) | EP1735068B1 (de) |
JP (1) | JP2007530273A (de) |
CN (1) | CN1960789B (de) |
BR (1) | BRPI0509474A (de) |
DE (1) | DE102004015714B3 (de) |
WO (1) | WO2005092464A1 (de) |
ZA (1) | ZA200608013B (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU2010260885B2 (en) * | 2009-06-17 | 2015-03-12 | Keio University | Prophylactic and/or therapeutic agent for dysmenorrhea |
US9156768B2 (en) | 2010-05-10 | 2015-10-13 | Evonik Degussa Gmbh | Isolation of acrylic acid by means of a distillation column having a side offtake |
Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
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DE102004005863A1 (de) * | 2004-02-05 | 2005-09-08 | Stockhausen Gmbh | Reaktor mit einem einen Einsatz aufweisenden Wärmetauscherbereich |
DE102006036177B4 (de) * | 2006-07-21 | 2013-05-08 | Evonik Degussa Gmbh | Vorrichtung und Verfahren zur Herstellung von Acrylsäure mit verminderter Autoxidationsneigung |
DE102006039205A1 (de) * | 2006-08-22 | 2008-03-20 | Stockhausen Gmbh | Auf nachwachsenden Rohstoffen basierende Acrylsäure und wasserabsorbierende Polymergebilde sowie Verfahren zu deren Herstellung mittels Dehydratisierung |
DE102013217386A1 (de) | 2013-09-02 | 2015-03-05 | Evonik Industries Ag | Verfahren zur Herstellung von Acrylsäure |
DE102014215438A1 (de) * | 2014-08-05 | 2016-02-11 | Basf Se | Kolonne zur thermischen Behandlung von fluiden Gemischen |
MX2018000232A (es) | 2015-07-08 | 2018-03-08 | Koch Glitsch Lp | Bandeja de valvula de contacto para una columna de transferencia de masa. |
AR104100A1 (es) * | 2016-03-21 | 2017-06-28 | Porta Hnos S A | Plantas de destilación de alcohol de cereales |
USD816189S1 (en) | 2016-06-07 | 2018-04-24 | Koch-Glitsch, Lp | Tray valve |
USD816188S1 (en) | 2016-06-07 | 2018-04-24 | Koch-Glitsch, Lp | Tray valve cover |
CN108164405A (zh) * | 2018-02-01 | 2018-06-15 | 南通鸿富达利化工有限公司 | 一种频哪酮粗品混合液分离装置 |
CN110433518A (zh) * | 2019-07-31 | 2019-11-12 | 常州大学 | 一种脉动浮阀传质元件 |
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DE19530291A1 (de) * | 1995-08-17 | 1997-02-20 | Basf Ag | Vorrichtung und Verfahren zum Stoffaustausch in Bodenkolonnen |
MY122671A (en) * | 1999-03-06 | 2006-04-29 | Basf Ag | Fractional condensation of a product gas mixture containing acrylic acid |
DE50003359D1 (de) * | 1999-03-06 | 2003-09-25 | Basf Ag | Verfahren zur herstellung von acrylsäure |
US7803969B2 (en) * | 2001-01-12 | 2010-09-28 | Evonik Stockhausen Gmbh | Continuous process for the production and purification of acrylic acid |
-
2004
- 2004-03-29 DE DE102004015714A patent/DE102004015714B3/de not_active Expired - Lifetime
-
2005
- 2005-03-29 US US11/547,109 patent/US20070262022A1/en not_active Abandoned
- 2005-03-29 BR BRPI0509474-7A patent/BRPI0509474A/pt not_active Application Discontinuation
- 2005-03-29 CN CN2005800173692A patent/CN1960789B/zh not_active Expired - Fee Related
- 2005-03-29 EP EP05735782.4A patent/EP1735068B1/de active Active
- 2005-03-29 WO PCT/EP2005/003271 patent/WO2005092464A1/de active Application Filing
- 2005-03-29 JP JP2007505482A patent/JP2007530273A/ja active Pending
-
2006
- 2006-09-27 ZA ZA200608013A patent/ZA200608013B/en unknown
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DE1192621B (de) * | 1962-12-20 | 1965-05-13 | Pintsch Bamag Ag | Siebboden fuer Stoffaustauschkolonnen mit grossem Durchmesser |
DE2305564A1 (de) * | 1972-02-07 | 1973-08-16 | Shell Int Research | Boden zum kontaktieren von fluessigkeit und gas |
US6641700B1 (en) * | 1999-03-09 | 2003-11-04 | Nippon Shokubai Co., Ltd. | Purifying apparatus possessing vapor dispersing device |
DE19929407C1 (de) * | 1999-06-26 | 2001-01-18 | Informations Und Prozestechnik | Stoffaustauschapparat |
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AU2010260885B2 (en) * | 2009-06-17 | 2015-03-12 | Keio University | Prophylactic and/or therapeutic agent for dysmenorrhea |
US9592213B2 (en) | 2009-06-17 | 2017-03-14 | National University Corporation Kumamoto University | Prophylactic and/or therapeutic agent for dysmenorrhea |
US9156768B2 (en) | 2010-05-10 | 2015-10-13 | Evonik Degussa Gmbh | Isolation of acrylic acid by means of a distillation column having a side offtake |
Also Published As
Publication number | Publication date |
---|---|
CN1960789A (zh) | 2007-05-09 |
BRPI0509474A (pt) | 2007-09-11 |
JP2007530273A (ja) | 2007-11-01 |
CN1960789B (zh) | 2011-08-10 |
EP1735068A1 (de) | 2006-12-27 |
ZA200608013B (en) | 2008-07-30 |
US20070262022A1 (en) | 2007-11-15 |
EP1735068B1 (de) | 2019-03-06 |
DE102004015714B3 (de) | 2005-12-15 |
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