M�Sl�M Film Stream Info zu Unitymedia- und Kabel-Produkten in NRW, BW oder Hessen
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The prior art regards merely the isolation and Dark Crimes Imdb dissociation of the Michael adducts as a possible solution to the problem cf. However, there is in many cases a particularly appropriate selection of the volume elements i. The dual-flow, or else trickle sieve, trays differ from the forced sieve trays in that they contain no drain segment. It is outstandingly suitable for preparing superabsorbents based on poly-sodium acrylate. For the aforementioned removals, one Filme Stream Seiten Legal more thermal separating processes as described at the outset are frequently employed. An analysis shows that this improvement can be attributed, among other factors, to the liquid phase in the bottom space 5 in the example The Birth Of A Nation 1915 only No further constituents were detected. However, they may Fußball Schauen have triple-flow and multiflow for example up to octuple-flow configuration. About Mighty Med Staffel 3 Discussion middot Grup Filme Turcesti nbsp 0 00 0 A first possibility is to reduce the tubular cross sections of the pipe lines of the separating space through which liquid phase containing meth acrylic monomers is conducted at the cost of a certain M�Sl�M Film Stream drop at the same volume flow rate and minimize the tube length. 
M�Sl�M Film Stream Despacito Po Polsku HD Video Video
Roja (1992) - Tamil Full Movie - Arvind Swamy, Madhoo - Full HD (1080p)The liquid phase to be heated in the direct circulation evaporator 1 is a mixture of bottoms liquid withdrawn from the bottom space 5 and of high boiler fraction which is withdrawn from the first collecting tray 10 completing the bottom space 5 of the separating column The temperature of the bottoms liquid is The vapor pressure is 1.
The temperature of the high boiler fraction is The biphasic mixture leaving the direct circulation evaporator 1 at a temperature of The pressure in the bottom space 5 and in the direct circulation evaporator 1 is 1.
The height of the separating column 28 a column for fractional condensation whose separating internals are only mass transfer trays; from bottom to top, these are initially dual-flow trays and then hydraulically sealed crossflow trays Thormann trays which are finally superseded by valve trays is The internal diameter of the separating column 28 in the region of the Thormann trays is 6.
The number of dual-flow trays is The forced circulation flash evaporator consists of a dissociation vessel, a heat exchanger, a pump and the accompanying pipelines.
The bottom effluent from the dissociation vessel is fed via a pipeline to a centrifugal pump which feeds it to a tube bundle heat exchanger. Subsequently, a portion of the heated liquid is recycled into the dissociation vessel via a pipeline.
The other portion of the heated liquid is fed under viscosity preferred , density or temperature control into a vessel to be described hereinbelow, in which methanol is mixed in.
Like the separating column 28 , the rectification column is insulated from the environment. The internal diameter of the rectification column over all dual-flow trays is a uniform 2.
Its height is 27 m. The dual-flow trays are arranged equidistantly mm in the rectification column. Viewed from bottom to top, the hole diameter of the first eight dual-flow trays is a uniform 25 mm hole arrangement corresponding to strict triangular pitch and the hole diameter of all subsequent dual-flow trays is a uniform 14 mm hole arrangement likewise corresponding to strict triangular pitch.
The feed of the bottoms liquid to be subjected to the dissociation is to the eighth dual-flow tray from the bottom.
The contents of the cycle gas are: 0. The dissociation gases forming in the dissociation vessel are conveyed into the attached rectification column by the support gas fed and rise therein in descending reflux liquid.
The composition of the quench liquid I is: A centrifugal drop separator is integrated into the bottom space 5 of the condensation column 28 and prevents droplets of the bottoms liquid being entrained upward out of the bottom space.
As already mentioned, the bottom space of the separating column 28 is completed at a column height like all heights, calculated from the column bottom of 7.
The free gas cross section is approx. The passages consist of circular orifices of a uniform diameter of 14 mm, with the punched burr pointing downward in the separating column.
The arrangement of the centers of the passage circles follows strict triangular pitch. The fifteenth dual-flow tray 12 is configured as a distributor tray.
For this purpose, two insert tubes DN having 40 drain drillholes diameter: 15 mm per insert tube are mounted above it. The first series of dual-flow trays is completed by a second collecting tray 14 chimney tray having 16 approx.
From this second collecting tray 14 , crude acrylic acid at a temperature of The liquid volume on the second collecting tray 14 is 10 m 3. The cooling medium is conveyed in countercurrent to the crystallizing mixture through the crystallizer from cooling disk to cooling disk.
However, It may also be conducted over the cooling plates divided into 2 or 3 parallel streams. The wiping of the cooling plates suppresses the formation of a crystal layer.
The crude acrylic acid having increased water content is conducted continuously pumped or controlled by overflows from back to front through the crystallizer.
The monophasic crude acrylic acid having increased water content thickens residence time from 0. The shaft which drives the wipers and passes through the centers of the cooling disks is sealed with water-washed stuffing box packings packing braids made of Teflon or graphite.
On the circumference of the cooling disks where it is not possible to wipe, a hollow profile e. These circumference heaters are flowed through in parallel by the second heat carrier.
The specific pressing force of the wipers perpendicular to the cooling surface in the installed state is from 1 to 10 N, preferably from 3 to 5 N, per cm of active wiping edge length.
In addition to the wipers, the shaft drives paddles there are advantageously two each in a symmetrical arrangement between two cooling disks and before the first and last cooling disk which bring about improved mixing.
The nature of the cooling plate surface and the alignment of the wipers are such that the distance of the wipers from the cooling plate surface at no point exceeds 6 mm it is favourable to operate with the aforementioned distance at no point exceeding 4 or 2 or 1 mm, or with the wipers being in contact at each point; it has been found to be particularly advantageous for there to be contact at the outer radius.
In the last section of the crystallizer in the conveying direction of the suspension preferably beyond the last cooling disk , the suspension is conducted via an attached tube appropriately mounted immersed; alternatively, the suspension may flow via an overflow weir into a stirred reservoir, whence the washing columns are charged to hydraulic melt-washing columns, as described in DE-A 10 and DE-A 10 , in order to separate the mother liquor from the suspension crystals.
The washing columns are charged with crystal suspension by means of a centrifugal pump or a rotary piston pump.
The control stream pump is likewise configured as a rotary piston pump or as a centrifugal pump having a regulating valve. The top pressure is generally up to 6 bar, usually from 0.
The filtration front is detected according to DE-A 10 by from 2 to 4 optical sensors. The washing front is controlled by means of temperature measurement in the crystal bed.
The total height of the crystal bed is typically from to mm, usually from to mm. The washing front is typically from 10 to mm, usually from 20 to mm, above the blade.
Useful melt circuit pumps are a centrifugal pump with product-side washing of the shaft seal slip-ring seal or a magnet-coupled pump with increased washing of the sliding bearings.
The melt circuit is stabilized by means of from to ppm by weight of MEHQ. Preference is given to washing the crystals removed from the 2nd or 3rd stage of the centrifuge with from 0.
Flushing and washing liquid are preferably molten crystals removed and washed by the centrifuge. The product space of the centrifuge is appropriately inertized with nitrogen or with a mixture of air and nitrogen.
The shaft seal is purged with gas e. Instead of recycling the mother liquor from a following purification stage into a preceding purification stage, it is also possible to recycle them together into the condensation column.
It is outstandingly suitable for preparing superabsorbents based on poly-sodium acrylate. The mother liquor removed in the washing columns is initially conducted into a heatable collecting vessel and from there into a tank.
The contents of this recycled mother liquor are as follows: The reflux from the Thormann tray region into the dual-flow tray region is via a distributor system integrated into the column.
Alternatively, reflux could also be effected by conducting the reflux liquid out of the condensation column below the lowermost Thormann tray by means of a pump and recycling it into the condensation column via two or more Insert tubes which are mounted above the uppermost dual-flow tray.
At this height, i. The Thormann trays are configured in such a way that the arrangement of the transport slots in the hoods of the Thormann trays in successive channels in the crossflow direction each generate a mutually opposed flow direction of the liquid.
The ratio of chimney surface area to slot exit surface area is 0. The chimney height and the height of the overflow weir are 40 mm.
The bottom clearance of the bubble-cap distance between lower edge of slot and tray is 10 mm. The slot height is 15 mm.
The angle between obliquely angled slot and longitudinal edge of the hood is 30 degrees. The maximum length of the longitudinal edge of the hood is mm.
In the peripheral region of the column, the hood length reduces to mm for reasons of adaptation to the roundness of the column. The distance between two hoods disposed on a line in the crossflow direction is 66 mm.
The drain surface area of the downcorner is 1. The breadth between the two lower longitidunal edges of a hood is 64 mm. At the height of the uppermost Thormann tray 20 , the separating column begins to narrow again conically.
The contents of the acid water are: The height of the overflow weir is 35 mm. The stream which is conducted out of the separating space with the highest proportion by weight of acrylic acid is the crude acrylic acid removed from the second collecting tray which has an acrylic acid content of The total volume of the separating space filled with liquid phase is The temperature of this liquid phase is, at least in places, The numbering of the mass transfer trays numbers from bottom to top in the separating column.
Total volume 21 Substantially everything is carried out as in the comparative example. This change is required in order, in the direct circulation evaporator 1 , to achieve the boiling temperature which falls in the bottom space 5 as a consequence of the changed composition of the bottoms liquid.
Table 2 which follows is the analog of table 1 for the example. An analysis shows that this improvement can be attributed, among other factors, to the liquid phase in the bottom space 5 in the example containing only A thermal separating process for removing at least one stream containing enriched meth acrylic monomers from a mixture containing methacrylic monomers, comprising the continuous steady-state operation of at least one thermal separating apparatus which comprises at least one separating space with or without separating internals, into which at least one stream containing meth acrylic monomers is conducted and out of which at least one stream containing meth acrylic monomers is conducted, with the proviso that.
A process as claimed in any of claims 1 to 4, wherein the at least one meth acrylic monomer is selected from the group consisting of acrolein, methacrolein, acrylic acid.
A process as claimed in any of claims 1 to 7, wherein the separating space comprises a separating column having mass transfer trays as separating internals.
A process as claimed in any of claims 1 to 8, wherein the circulation heat exchanger is a circulation evaporator. A process as claimed in any of claims 1 to 9, wherein the circulation heat exchanger is a direct circulation evaporator.
A process as claimed in claim 8, wherein the mass transfer trays of the separating column, from bottom to top, are initially dual-flow trays, then hydraulically sealed crossflow trays and finally valve trays.
Justia Patents US Patent Application for Thermal separating process for removing at least one stream containing enriched meth acrylic monomers Patent Application Application Thermal separating process for removing at least one stream containing enriched meth acrylic monomers.
The pressure at the top of the column 28 is 1. Patent History. Current U. Justia Legal Resources. Find a Lawyer. Law Students. US Federal Law.
US State Law. Drainpipes equipped with weirs conduct the reflux from tray to tray. Frequently, they have double-flow configuration. However, they may also have triple-flow and multiflow for example up to octuple-flow configuration.
Mass transfer trays on which there is equilibrium between descending liquid and rising vapor are referred to as theoretical plates.
This term can be applied to all other separating internals which are suitable for countercurrent distillations rectifications such as structured packings and random packings and to other thermal separating procedures such as sorption and extraction.
In the case of the latter too, the separating internals mentioned bring about an increase in the exchange surface between then two liquid phases.
It is therefore appropriate to refer generally to theoretical plates. A theoretical plate is defined as the spatial unit which brings about enrichment in accordance with the thermodynamic equilibrium.
The aim of a thermal separating process for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers is firstly a very high degree of enrichment of the meth acrylic monomers in the removed stream containing enriched meth acrylic monomers and secondly a very high space-time yield of this removed stream.
A disadvantage of the thermal separating processes described at the outset is that those measures which, under otherwise constant boundary conditions, increase the degree of enrichment normally at the same time reduce the space-time yield for example an increase in the number of theoretical plates typically improves the degree of enrichment; but an increase in the number of theoretical plates under otherwise identical boundary conditions normally decreases the space-time yield.
It is an object of the present invention to break through the aforementioned relationship and to provide a thermal separating process as described at the outset for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers, in which the degree of enrichment and space-time yield are at the same time increased.
The background to the procedure according to the invention is the fact that methacrylic monomers form oligomers or polymers Michael adducts by simple or multiple Michael addition.
A disadvantage of the Michael adduct formation of meth acrylic monomers is that they are also effected in the course of thermal separating processes for removing a stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers, thus reducing both the degree of enrichment and the space-time yield.
The prior art regards merely the isolation and subsequent dissociation of the Michael adducts as a possible solution to the problem cf.
Detailed investigations have led to the process according to the Invention as a further contribution to the solution to the problem.
This contribution to the solution to the problem takes into account that a Michael adduct of meth acrylic monomers is formed substantially only in the liquid phase.
In other words, when care is taken in continuously operated thermal separating processes for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers in steady-state operation that the residence time of the meth acrylic monomers in the liquid phase is particularly low where temperature and proportion by mass of meth acrylic monomers in the liquid phase are high, the disadvantageous Michael adduct formation of meth acrylic monomers in the course of such thermal separating processes can be prevented to a certain extent.
A suitable measure in this regard is a mean overall residence time of the meth acrylic monomers which they have in the liquid phase in the separating space in the thermal separating process and is calculated in an appropriate manner from individual residence times.
To this end, the separating space is divided into n individual volume elements. The size and number n of these volume elements is substantially insignificant in other words, the individual volume elements may either be of equal size or have different volumes.
Finally, it is necessary to sum over all volume elements l which contain liquid phase. Deadspace volume elements l are not to be included in the sum in that they are substantially not involved in the separating process.
Deadspace volume elements essentially take no part in the exchange processes which bring about the separating action in the separating process according to the invention.
These volume elements are substantially isolated volume elements which fill once with liquid phase and contain substantially one and the same liquid phase over the time.
In principle, deadspace volume elements are to be very substantially avoided in the process according to the invention, especially because they have an increased probability of the commencement of free-radical polymerization of the meth acrylic monomers present therein.
In other words, the number of theoretical plates is not impaired by the process according to the invention. In general, X:Y in the process according to the invention will not exceed The procedure according to the invention is advantageous in particular when the total volume V filled with liquid phase in the separating space has a large volume.
In general, V will not be more than m 3. These temperatures are generally not capable of achieving significant dissociative action, since this requires that the dissociation products are continuously removed from the dissociation equilibrium.
The process according to the invention is suitable, inter alia, to the rectificative processes described in the documents EP-A and EP-A for purifying crude meth acrylic acid, to the processes for fractional condensation described in the documents DE-A 19 Usually, the separating space in the aforementioned processes and in the process according to the invention quite generally includes at least one circulation heat exchanger and at least one column with or without separating internals.
Since absorptive removals generally proceed exothermically, the at least one circulation heat exchanger in this connection generally fulfills the purpose of heat removal.
This is normally effected by an indirect route by means of a cold carrier coolant which never enters the separating space.
In other words, only one of the two spatial sides of the indirect heat exchanger is a constituent of the separating space. The other is outside and conducts the cold carrier, The streams are conveyed through the spatial side of the heat exchanger belonging to the separating space typically by means of at least one pump.
In the majority of the thermal removals which differ from absorptive removal, heat is supplied to the separating space via the circulation heat exchanger.
In most cases, this is likewise effected by an indirect route by means of a heat carrier which never enters the separating space. The other is outside and conducts the heat carrier.
Frequently, sufficient heat is supplied that boiling phenomena occur in the spatial side of the heat exchanger belonging to the separating space.
In this case, the circulation heat exchanger is referred to as a circulation evaporator. Especially when the thermal separating process according to the invention is a rectification, the circulation heat exchanger used is a circulation evaporator.
In principle, the indirect circulation heat exchangers used in the process according to the invention may be all known indirect heat exchanger types.
Preference is given to selecting them in such a way that the liquid phase volume retained therein is minimal. Useful circulation evaporators are, for example, Robert evaporators natural circulation evaporators integrated into the separating column as outlined in FIG.
However, the circulation evaporator may also be a forced circulation evaporator installed outside the separating column as shown by FIG. It will be appreciated that the circulation evaporator used may also be a forced circulation flash evaporator, as shown schematically by FIG.
In contrast to the forced circulation evaporator, the forced circulation flash evaporator is separated from the separating column by a throttle apparatus.
A portion of the liquid contents of the separating column at a pressure P x is continuously withdrawn and pumped into the feeds of, for example, a tube evaporator tube bundle heat exchanger by means of a circulation pump.
Around the internal tubes of the tube evaporator flows a heat carrier, for example heating vapor generally steam under pressure whose temperature is above the temperature of the liquid contents of the separating column.
On the path through the inlet and outlet tubes of the tube evaporator, the separating column liquid withdrawn is heated by indirect heat exchange to a temperature T y which is above the temperature of the liquid contents of the separating column.
A throttle apparatus separates tube evaporator and separating column on the pressure side and, by suitable choice of the circulation pump output, allows a throttle pressure P y to be set which is above P x and is above the boiling pressure P y corresponding to the temperature T y of the separating column liquid withdrawn.
The above measures suppress boiling of the portion of separating column liquid pumped by circulation in the tubes of the tube evaporator.
The proportion of the separating column liquid pumped by circulation is actually superheated in the tubes of the tube evaporator with respect to the pressure P x above the liquid contents of the separating column and the boiling process is thus shifted to the passage side of the throttle apparatus i.
The passage of the superheated liquid through the throttle apparatus into the separating column may then be directly into the liquid contents of the separating column the separating column bottoms.
Under these conditions, the temperature of the liquid contents of the separating column bottoms regularly corresponds to the boiling temperature T x corresponding to the pressure P x above the bottoms liquid.
However, the superheated liquid may in principle also pass through the throttle apparatus into the separating column above the liquid level of the separating column bottoms.
Under these conditions, the temperature of the liquid contents of the separating column bottoms is regularly below the boiling temperature T x corresponding to the pressure P x above the bottoms liquid.
It is essential that the evaporative action of the tube evaporator installed outside the separating column does not occur until within the separating column, i.
However, the circulation evaporator may also be a direct circulation evaporator, as shown by way of example in FIG.
Subsequently, the entire mixture 10 is recycled into the bottoms liquid recycling does not have to be immersed of the separating column and the gas mixture which ascends therefrom is fractionally condensed ascending into itself.
The liquids withdrawn from the separating column are conveyed by means of pumps 4 , 5 , 3 is the bottom product withdrawal and 7 is the level of the bottoms liquid.
The direct circulation evaporator is generally free of separating internals and is of cylindrical geometry. In principle, the gas and liquid phase from the direct circulation evaporator may also be recycled spatially separated into the separating column.
Such a direct circulation evaporator is shown schematically by FIG. The numbers have the same definition as in FIG.
The separating column may either be free of separating internals, or contain separating internals, in which case useful separating internals for carrying out the process according to the invention are in principle all separating internals already mentioned in this document themselves or optionally together with other separating internals.
Useful bed-type packings are, for example, Raschig glass rings, saddles, wire mesh rings, V2A spirals, Pall rings and Stedman bodies, and also random packings of the second, third and fourth generation.
Useful insert-type packings whose diameter is substantially equal to the column internal diameter are structured packings of highly differing types.
The number of theoretical plates is appropriately from 15 to 30 and preferably The evaporator is appropriately a direct circulation evaporator as described above.
When an acid water quench is also integrated into the condensation column, useful separating internals for this region of the condensation column are preferably valve trays, as described by DE-A , DE-A and DE-A 10 In other words, the inventive aim can be achieved, inter alia, by, with substantially equal streams and theoretical plates, minimizing the total amount of liquid phase retained in the separating space in the steady state, and in particular in those volume elements in which the liquid phase has a particularly high temperature and whose minimization does not reduce the number of theoretical plates.
Among others, the possibilities which follow are available. A first possibility is to reduce the tubular cross sections of the pipe lines of the separating space through which liquid phase containing meth acrylic monomers is conducted at the cost of a certain pressure drop at the same volume flow rate and minimize the tube length.
In a fractional condensation to be carried out as described, it is advantageous in the context of the present invention when, apart from a direct circulation evaporator, no further circulation heat exchanger belongs to the separating space.
In other words, unlike the recommendation of FIG. According to the invention, a direct circulation evaporator will preferably not be configured as in FIG.
At the same time, the cross section of the direct circulation evaporator at the same circulation rate the direct circulation evaporator functions at the same time as a direct cooler for the product gas mixture of the partial oxidation; for reasons relating to heat balance, a certain minimum circulation rate is required will be kept at a minimum, in order thus to keep to a minimum the total amount of liquid phase retained in the system of the separating space.
When the separating internals of the separating space are mass transfer trays, these mass transfer trays will in accordance with the invention advantageously be sieve trays, more preferably trickle sieve trays dual-flow trays.
Since the latter have no overflow weirs, they can be operated with a particularly low liquid level and are preferred in accordance with the invention over hydraulically sealed crossflow trays.
The latter will be used only when the separating action achievable with dual-flow trays is not adequate. When the separating space includes collecting trays for example as a constituent of the separating column , from which, for example, liquid stream removed can be conducted out of the separating space for example into the storage tank or into the circulation heat exchanger , it will be operated in accordance with the invention with a very low liquid level.
This is made possible, for example, by applying displacement bodies to the collecting trays. These allow an increased liquid level at reduced liquid volume.
An alternative solution is offered by DE-A in the form of collecting trays having slopes. It has been found that appropriate displacement bodies are generally also advantageous in the process according to the invention in the bottom segments bottom spaces of the separating columns.
These are generally those spatial fractions which, in a geometric sense, are below the lowermost separating internals. In particular in the case of a rectification as the separating process according to the invention, bottoms liquid is regularly removed from the bottom segments, in order to feed it, for example, to forced circulation heat exchangers.
At the same time, the bottoms liquid is generally in a state of boiling. In order to prevent the pump required for forced circulation in the forced circulation heat exchanger from drawing too much gas, for example in the event of operating faults this generally reduces the conveying output of the pump and in unfavorable cases can lead to its destruction, since the pump is normally configured only to convey liquid , a safety liquid head, a safety liquid level, is typically established in the bottom segment.
This safety head is advantageously achievable in accordance with the invention with reduced bottom volume by introducing displacement bodies in the bottom space or contracting the bottom space, as shown, for example, by FIG.
It will be appreciated that this reduction of the bottom volume in the process according to the invention can be applied quite generally.
It is to be preferred in accordance with the invention in any case over those solutions as shown by FIG. Pumps used in accordance with the invention are appropriately selected in such a way that they retain a very small amount of liquid.
The determination of the temperatures T l in the process according to the invention is possible in a simple manner by experimental determination for example by means of thermoelements mounted in a suitable manner.
In principle, the selection of the volume elements l in the process according to the invention is arbitrary and has substantially no effect on the result of t ort.
However, there is in many cases a particularly appropriate selection of the volume elements i. In the case of mass transfer trays with forced flow, the volume element l selected is appropriately that volume element which includes the liquid level on the mass transfer tray and the feed to the mass transfer tray below, as shown schematically in FIG.
By means of chemical content analysis, m l finally results in m sl. The latter can be effected, for example, by taking a small sample continuously at the point having the number 7 in FIG.
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Seriale Turcesti oficial grup 3 English Seriale noi. Seriale turcesti lista Seriale Turcesti. About middot Discussion middot Grup Filme Turcesti nbsp 0 00 0 Top ul celor mai bune seriale Netflix l va deschide noul proiect pilot alc tuit din 18 filme scurte de anima ie cu elemente tiin ifico fantastice i subiecte complet diferite.
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In the crossflow trays, viewed over the entire flow area, the liquid is conducted transversely over the tray from feed to drain.
In general, crossflow trays have a single-flow configuration. In other words, feed and drain are disposed on opposite sides of the tray.
However, they may also have a double-flow or else more than double-flow configuration. In this case, the feed may be disposed, for example, in the middle and a drain on each of the opposite sides of the mass transfer tray.
In other words, the forced liquid flow in sieve trays is achieved by the sieve trays having, in addition to the passages for the ascending gas or vapor phase, at least one downcorner drain , through which the liquid, irrespective of the flow path of the vapor, flows from the upper tray to the lower tray feed.
The liquid flows, for example, in transverse flow over the tray from at least one feed to at least one drain, in which case the feed pipe and drainpipe guarantee the liquid seal and the desired liquid height on the tray.
Frequently especially in the case of low column diameters , the sieve trays with forced liquid flow have a single-flow configuration. In this case, the feed may be disposed, for example, in the middle and one drain on each of the opposite sides of the mass transfer tray.
Such sieve trays are to be referred to hereinbelow as forced sieve trays. In these trays, trickle-through of the liquid which reduces the separating action is not, as in the case of hydraulically sealed crossflow trays, prevented by chimneys, into which the passages continue, but rather a minimum vapor loading is required for this purpose.
The vapor ascends through the passages and bubbles through the liquid layer maintained by the drainpipe. The dual-flow, or else trickle sieve, trays differ from the forced sieve trays in that they contain no drain segment.
The absence of drain segments downcorners in the dual-flow trays results in the ascending gas and the liquid descending in the separating column passing through the same passages of the tray.
As in the case of forced sieve trays, a minimum vapor loading is also required in the case of dual-flow trays, in order to achieve appropriate separating action.
When the vapor loading is significantly lower, ascending gas and descending reflux move past each other substantially without exchange and the tray is at risk of running dry.
In other words, in the case of dual-flow trays too, a lower limiting rate has to be present so that a certain liquid layer is maintained on the tray, in order to allow the tray to work.
In the normal working range, the liquid in dual-flow trays trickles through the passages from tray to tray, and the continuous gas phase between the trays is interspersed by a divided liquid phase.
Compared to sieve trays, It is characteristic of hydraulically sealed crossflow trays that they cannot run dry when the column is shut down, disregarding the tiny emptying drillhole its cross section is normally more than times smaller than the total cross section of the passages which each crossflow tray has for reasons of utility.
This results from the fact that the passages of hydraulically sealed crossflow trays are not chimneyless drillholes, as is the case in sieve trays.
Rather, each passage opens into a chimney which prevents the tray from running dry. Above the chimney, vapor deflecting hoods bubble-caps are mounted which are immersed in the accumulated tray liquid.
Frequently, the vapor deflecting hoods are slotted or serrated at their edges i. The vapor stream ascending through the passage is deflected by the vapor deflecting hoods and flows parallel to the tray, i.
The vapor bubbles leaving adjacent hoods which are generally distributed equidistantly over the tray form a froth layer in the accumulated liquid.
Drainpipes or drain segments which leave trays, generally to the left or right in alternation, supported by weirs, control the liquid level of the mass transfer trays and feed the liquid to the tray below.
It is essential for the hydraulic sealing action that the drainpipes or drain segments of the upper tray are immersed in the accumulated liquid of the tray below.
There are preferably no feed weirs. Bubble-caps which can be adjusted in height allow adaptation to the flow conditions and the equalization of the immersion depths in the event of production irregularities, so that all bubble-caps of the tray have uniform gas flow.
Depending on the design and arrangement of the bubble-caps, the hydraulically sealed crossflow trays having single-flow configuration are divided, for example, into round bubble-cap trays passage, chimney and bubble-cap are round , tunnel-cap trays passage, chimney and bubble-cap are rectangular, the bubble-caps are arranged in succession with the longer rectangular edge aligned parallel to the crossflow direction of the liquid and Thormann trays passage, chimney and bubble-cap are rectangular, the bubble-caps are arranged in succession with the longer rectangular edge at right angles to the crossflow direction of the liquid.
In this document, valve trays are crossflow trays which have tray drillholes having limited-stroke plate, ballast or lifting valves floating flaps which adapt the size of the vapor passage to the particular column loading.
The ascending gas stream is deflected, flows parallel to the tray into the accumulated reflux liquid and forms a froth layer.
Drainpipes equipped with weirs conduct the reflux from tray to tray. Frequently, they have double-flow configuration. However, they may also have triple-flow and multiflow for example up to octuple-flow configuration.
Mass transfer trays on which there is equilibrium between descending liquid and rising vapor are referred to as theoretical plates.
This term can be applied to all other separating internals which are suitable for countercurrent distillations rectifications such as structured packings and random packings and to other thermal separating procedures such as sorption and extraction.
In the case of the latter too, the separating internals mentioned bring about an increase in the exchange surface between then two liquid phases.
It is therefore appropriate to refer generally to theoretical plates. A theoretical plate is defined as the spatial unit which brings about enrichment in accordance with the thermodynamic equilibrium.
The aim of a thermal separating process for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers is firstly a very high degree of enrichment of the meth acrylic monomers in the removed stream containing enriched meth acrylic monomers and secondly a very high space-time yield of this removed stream.
A disadvantage of the thermal separating processes described at the outset is that those measures which, under otherwise constant boundary conditions, increase the degree of enrichment normally at the same time reduce the space-time yield for example an increase in the number of theoretical plates typically improves the degree of enrichment; but an increase in the number of theoretical plates under otherwise identical boundary conditions normally decreases the space-time yield.
It is an object of the present invention to break through the aforementioned relationship and to provide a thermal separating process as described at the outset for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers, in which the degree of enrichment and space-time yield are at the same time increased.
The background to the procedure according to the invention is the fact that methacrylic monomers form oligomers or polymers Michael adducts by simple or multiple Michael addition.
A disadvantage of the Michael adduct formation of meth acrylic monomers is that they are also effected in the course of thermal separating processes for removing a stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers, thus reducing both the degree of enrichment and the space-time yield.
The prior art regards merely the isolation and subsequent dissociation of the Michael adducts as a possible solution to the problem cf.
Detailed investigations have led to the process according to the Invention as a further contribution to the solution to the problem.
This contribution to the solution to the problem takes into account that a Michael adduct of meth acrylic monomers is formed substantially only in the liquid phase.
In other words, when care is taken in continuously operated thermal separating processes for removing at least one stream containing enriched meth acrylic monomers from a mixture containing meth acrylic monomers in steady-state operation that the residence time of the meth acrylic monomers in the liquid phase is particularly low where temperature and proportion by mass of meth acrylic monomers in the liquid phase are high, the disadvantageous Michael adduct formation of meth acrylic monomers in the course of such thermal separating processes can be prevented to a certain extent.
A suitable measure in this regard is a mean overall residence time of the meth acrylic monomers which they have in the liquid phase in the separating space in the thermal separating process and is calculated in an appropriate manner from individual residence times.
To this end, the separating space is divided into n individual volume elements. The size and number n of these volume elements is substantially insignificant in other words, the individual volume elements may either be of equal size or have different volumes.
Finally, it is necessary to sum over all volume elements l which contain liquid phase. Deadspace volume elements l are not to be included in the sum in that they are substantially not involved in the separating process.
Deadspace volume elements essentially take no part in the exchange processes which bring about the separating action in the separating process according to the invention.
These volume elements are substantially isolated volume elements which fill once with liquid phase and contain substantially one and the same liquid phase over the time.
In principle, deadspace volume elements are to be very substantially avoided in the process according to the invention, especially because they have an increased probability of the commencement of free-radical polymerization of the meth acrylic monomers present therein.
In other words, the number of theoretical plates is not impaired by the process according to the invention. In general, X:Y in the process according to the invention will not exceed The procedure according to the invention is advantageous in particular when the total volume V filled with liquid phase in the separating space has a large volume.
In general, V will not be more than m 3. These temperatures are generally not capable of achieving significant dissociative action, since this requires that the dissociation products are continuously removed from the dissociation equilibrium.
The process according to the invention is suitable, inter alia, to the rectificative processes described in the documents EP-A and EP-A for purifying crude meth acrylic acid, to the processes for fractional condensation described in the documents DE-A 19 Usually, the separating space in the aforementioned processes and in the process according to the invention quite generally includes at least one circulation heat exchanger and at least one column with or without separating internals.
Since absorptive removals generally proceed exothermically, the at least one circulation heat exchanger in this connection generally fulfills the purpose of heat removal.
This is normally effected by an indirect route by means of a cold carrier coolant which never enters the separating space.
In other words, only one of the two spatial sides of the indirect heat exchanger is a constituent of the separating space.
The other is outside and conducts the cold carrier, The streams are conveyed through the spatial side of the heat exchanger belonging to the separating space typically by means of at least one pump.
In the majority of the thermal removals which differ from absorptive removal, heat is supplied to the separating space via the circulation heat exchanger.
In most cases, this is likewise effected by an indirect route by means of a heat carrier which never enters the separating space.
The other is outside and conducts the heat carrier. Frequently, sufficient heat is supplied that boiling phenomena occur in the spatial side of the heat exchanger belonging to the separating space.
In this case, the circulation heat exchanger is referred to as a circulation evaporator. Especially when the thermal separating process according to the invention is a rectification, the circulation heat exchanger used is a circulation evaporator.
In principle, the indirect circulation heat exchangers used in the process according to the invention may be all known indirect heat exchanger types.
Preference is given to selecting them in such a way that the liquid phase volume retained therein is minimal. Useful circulation evaporators are, for example, Robert evaporators natural circulation evaporators integrated into the separating column as outlined in FIG.
However, the circulation evaporator may also be a forced circulation evaporator installed outside the separating column as shown by FIG.
It will be appreciated that the circulation evaporator used may also be a forced circulation flash evaporator, as shown schematically by FIG.
In contrast to the forced circulation evaporator, the forced circulation flash evaporator is separated from the separating column by a throttle apparatus.
A portion of the liquid contents of the separating column at a pressure P x is continuously withdrawn and pumped into the feeds of, for example, a tube evaporator tube bundle heat exchanger by means of a circulation pump.
Around the internal tubes of the tube evaporator flows a heat carrier, for example heating vapor generally steam under pressure whose temperature is above the temperature of the liquid contents of the separating column.
On the path through the inlet and outlet tubes of the tube evaporator, the separating column liquid withdrawn is heated by indirect heat exchange to a temperature T y which is above the temperature of the liquid contents of the separating column.
A throttle apparatus separates tube evaporator and separating column on the pressure side and, by suitable choice of the circulation pump output, allows a throttle pressure P y to be set which is above P x and is above the boiling pressure P y corresponding to the temperature T y of the separating column liquid withdrawn.
The above measures suppress boiling of the portion of separating column liquid pumped by circulation in the tubes of the tube evaporator.
The proportion of the separating column liquid pumped by circulation is actually superheated in the tubes of the tube evaporator with respect to the pressure P x above the liquid contents of the separating column and the boiling process is thus shifted to the passage side of the throttle apparatus i.
The passage of the superheated liquid through the throttle apparatus into the separating column may then be directly into the liquid contents of the separating column the separating column bottoms.
Under these conditions, the temperature of the liquid contents of the separating column bottoms regularly corresponds to the boiling temperature T x corresponding to the pressure P x above the bottoms liquid.
However, the superheated liquid may in principle also pass through the throttle apparatus into the separating column above the liquid level of the separating column bottoms.
Under these conditions, the temperature of the liquid contents of the separating column bottoms is regularly below the boiling temperature T x corresponding to the pressure P x above the bottoms liquid.
It is essential that the evaporative action of the tube evaporator installed outside the separating column does not occur until within the separating column, i.
However, the circulation evaporator may also be a direct circulation evaporator, as shown by way of example in FIG. Subsequently, the entire mixture 10 is recycled into the bottoms liquid recycling does not have to be immersed of the separating column and the gas mixture which ascends therefrom is fractionally condensed ascending into itself.
The liquids withdrawn from the separating column are conveyed by means of pumps 4 , 5 , 3 is the bottom product withdrawal and 7 is the level of the bottoms liquid.
The direct circulation evaporator is generally free of separating internals and is of cylindrical geometry. In principle, the gas and liquid phase from the direct circulation evaporator may also be recycled spatially separated into the separating column.
Such a direct circulation evaporator is shown schematically by FIG. The numbers have the same definition as in FIG.
The separating column may either be free of separating internals, or contain separating internals, in which case useful separating internals for carrying out the process according to the invention are in principle all separating internals already mentioned in this document themselves or optionally together with other separating internals.
Useful bed-type packings are, for example, Raschig glass rings, saddles, wire mesh rings, V2A spirals, Pall rings and Stedman bodies, and also random packings of the second, third and fourth generation.
Useful insert-type packings whose diameter is substantially equal to the column internal diameter are structured packings of highly differing types.
The number of theoretical plates is appropriately from 15 to 30 and preferably The evaporator is appropriately a direct circulation evaporator as described above.
When an acid water quench is also integrated into the condensation column, useful separating internals for this region of the condensation column are preferably valve trays, as described by DE-A , DE-A and DE-A 10 In other words, the inventive aim can be achieved, inter alia, by, with substantially equal streams and theoretical plates, minimizing the total amount of liquid phase retained in the separating space in the steady state, and in particular in those volume elements in which the liquid phase has a particularly high temperature and whose minimization does not reduce the number of theoretical plates.
Among others, the possibilities which follow are available. A first possibility is to reduce the tubular cross sections of the pipe lines of the separating space through which liquid phase containing meth acrylic monomers is conducted at the cost of a certain pressure drop at the same volume flow rate and minimize the tube length.
In a fractional condensation to be carried out as described, it is advantageous in the context of the present invention when, apart from a direct circulation evaporator, no further circulation heat exchanger belongs to the separating space.
In other words, unlike the recommendation of FIG. According to the invention, a direct circulation evaporator will preferably not be configured as in FIG.
At the same time, the cross section of the direct circulation evaporator at the same circulation rate the direct circulation evaporator functions at the same time as a direct cooler for the product gas mixture of the partial oxidation; for reasons relating to heat balance, a certain minimum circulation rate is required will be kept at a minimum, in order thus to keep to a minimum the total amount of liquid phase retained in the system of the separating space.
When the separating internals of the separating space are mass transfer trays, these mass transfer trays will in accordance with the invention advantageously be sieve trays, more preferably trickle sieve trays dual-flow trays.
Since the latter have no overflow weirs, they can be operated with a particularly low liquid level and are preferred in accordance with the invention over hydraulically sealed crossflow trays.
The latter will be used only when the separating action achievable with dual-flow trays is not adequate. When the separating space includes collecting trays for example as a constituent of the separating column , from which, for example, liquid stream removed can be conducted out of the separating space for example into the storage tank or into the circulation heat exchanger , it will be operated in accordance with the invention with a very low liquid level.
This is made possible, for example, by applying displacement bodies to the collecting trays. These allow an increased liquid level at reduced liquid volume.
An alternative solution is offered by DE-A in the form of collecting trays having slopes. It has been found that appropriate displacement bodies are generally also advantageous in the process according to the invention in the bottom segments bottom spaces of the separating columns.
These are generally those spatial fractions which, in a geometric sense, are below the lowermost separating internals. In particular in the case of a rectification as the separating process according to the invention, bottoms liquid is regularly removed from the bottom segments, in order to feed it, for example, to forced circulation heat exchangers.
At the same time, the bottoms liquid is generally in a state of boiling. In order to prevent the pump required for forced circulation in the forced circulation heat exchanger from drawing too much gas, for example in the event of operating faults this generally reduces the conveying output of the pump and in unfavorable cases can lead to its destruction, since the pump is normally configured only to convey liquid , a safety liquid head, a safety liquid level, is typically established in the bottom segment.
This safety head is advantageously achievable in accordance with the invention with reduced bottom volume by introducing displacement bodies in the bottom space or contracting the bottom space, as shown, for example, by FIG.
It will be appreciated that this reduction of the bottom volume in the process according to the invention can be applied quite generally.
It is to be preferred in accordance with the invention in any case over those solutions as shown by FIG. Pumps used in accordance with the invention are appropriately selected in such a way that they retain a very small amount of liquid.
The determination of the temperatures T l in the process according to the invention is possible in a simple manner by experimental determination for example by means of thermoelements mounted in a suitable manner.
In principle, the selection of the volume elements l in the process according to the invention is arbitrary and has substantially no effect on the result of t ort.
However, there is in many cases a particularly appropriate selection of the volume elements i. In the case of mass transfer trays with forced flow, the volume element l selected is appropriately that volume element which includes the liquid level on the mass transfer tray and the feed to the mass transfer tray below, as shown schematically in FIG.
By means of chemical content analysis, m l finally results in m sl. The latter can be effected, for example, by taking a small sample continuously at the point having the number 7 in FIG.
The tracer introduction point would appropriately be the point having the number 8 in FIG. In the case of dual-flow trays, it is possible to proceed in a corresponding manner.
The volume element l selected here is appropriately that volume element which includes the liquid level on the mass transfer tray and the space below the mass transfer tray up to the start of the surface of the liquid level of the next mass transfer tray.
The amount of liquid fed is conducted out of this collecting tray, the corresponding flow rate is determined and the liquid is subsequently recycled immediately above the sieve tray cf.
The amount of liquid on the dual-flow tray may be determined, for example, by means of a pressure differential meter according to FIG.
The amount of liquid between two dual-flow trays can be determined by simultaneously sealing both dual-flow trays and determining the amount of liquid collecting on the lower tray.
By means of chemical analysis, m l finally gives m sl. In complete agreement, m sl in the column bottom results from the bottoms level amount calculated from effluent and analysis of the composition of the bottoms liquid.
The same applies to the circulation pump, and the circulation heat exchanger can be treated likewise. Column sections having bed-type packings or insert-type packings can be treated in a similar manner to mass transfer tray volume elements.
However, the m sl and m l values within a separating column can also be determined semi empirically in very good approximation cf.
Klaus Hoppe and Dr. To this end, the particular tray temperature is initially determined, for example, over the different mass transfer trays.
The composition is then determined of feeds and effluents from the separating column. Raoult's law vapor-liquid equilibrium combined with mass-energy balances are then used to calculate the concentration profiles in the column.
The required liquid and gas flow rates then result from these. The m sl values can be determined as follows. In separate experiments gas flows from below and liquid is applied from above , the hydrodynamic behavior of the separating internals, for example of the mass transfer trays, is initially determined.
These give m l values, from which the m sl values finally follow by means of the concentration profiles.
The surprising result of the procedure according to the invention is that a reduction of t ort under otherwise substantially constant boundary conditions allows both the space-time yield and the degree of enrichment to be improved.
