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    • 专利摘要:
    An improved process for separating normal paraffins from a feed stream containing a mixture of normal paraffins and isoparaffins. The general process comprises the steps of contacting the feed stream with an adsorbent comprising a crystalline aluminosilicate thereby adsorbing normal paraffins and subsequently contacting the adsorbent with a desorbent material to remove the adsorbed normal paraffins. The improvement resides in a method of fractionating and recycling a desorbent material for re-use in the process in a manner that reduces total fractionation energy requirements. The method is particularly suitable when two desorbent materials are used in the process.
    公开号:SU984401A3
    申请号:SU762421353
    申请日:1976-11-19
    公开日:1982-12-23
    发明作者:Джозеф Байсер Герберт
    申请人:Юоп Инк (Фирма)；
    IPC主号:
    专利说明:

    paraffinic hydrocarbons at 40–250 ° C and pressures of 11–35 atm and extraction of an extract stream containing normal paraffinic hydrocarbons, a cleansing agent and a desorbent, followed by the flow of the extract into the first fractionation. devices to produce a first head stream containing a mixture of a cleansing agent and a desorbent, and a first bottoms fraction containing normal paraffinic hydrocarbons, a raffinate stream into the second fractionation devices to produce a second head stream, derived from a mixture of cleansing agent and desorbent, and a second bottoms the residue containing isoparaffin hydrocarbons, separation of the mixture of cleaning agent and desorbent in the third fractionation devices with obtaining the third head desorbent stream and. the third VAT residue — the cleaning agent — and recycling them to the desorption and cleaning zones and carrying out the separation process with periodic displacement of the functional zones in the direction of the liquid flow inside the column through the mass of adsorbent and continuous flows of the obtained extract and raffinate G2. The purpose of the invention is to reduce the energy consumption of the process.  The delivered material is obtained by separating normal paraffin hydrocarbons from a mixture containing isoparaffinic hydrocarbons by directing the feedstock in the liquid phase to a column filled with an adsorbent selective for normal paraffinic hydrocarbons and having at least three functional zones arranged in series and interconnected including end zones providing continuous cyclic flow in one direction in the following order: the adsorption zone located between the incoming Otok raw y.  the upper boundary and the effluent of the resulting raffinate at the lower boundary; a purification zone located above the adsorption zone located between the output stream of the obtained extract at the upper boundary and the output stream of the raw material at the lower boundary, and having an incoming stream of cleaning agent located above the incoming stream of the raw material; the desorption zone located above the purification zone is located between the incoming desorbent stream at the border and the extract stream at the lower boundary, with the supply of a rafinate-type cleansing agent to the purification zone, to the process of adsorption of normal paraffin hydrocarbons at 40-250 0 and a pressure of 1-35 atm and output of a raffinate stream containing isoparaffin hydrocarbons, a cleansing agent and a desorbent, to the desorption-desorbent zone with the process of desorption of normal paraffin hydrocarbons levodorods at 40–250С and a pressure of 1–35 atm and discharge of an extract stream containing normal paraffinic hydrocarbons, a cleansing agent and a desorbent, followed by directing the extract stream to the first fractionation devices to produce a first head stream containing a mixture of cleansing agent and desorbent, with the selection of side product withdrawn above the feed point of the raw material, and the first bottom fraction containing normal paraffin hydrocarbons, the raffinate stream into the second fractionation devices to produce the second g a final stream consisting of a mixture of a cleansing agent and a desorbent, with side stream withdrawal above the feed point, and a second bottoms containing isoparaffin hydrocarbons, separating the mixture of side batches in the third fractionation devices with the third head desorbent stream and the third bottoms — cleaning agent — and recycling the mixture of the third, second, and first head streams to the desorption zone. and in the purification zone of the third VAT residue, while the separation in the first and second fractionation devices is carried out with the selection of side shoulder straps withdrawn above the feed point of the feed fractionation devices, with the mixture of side streams fed into the third fractionation devices and recycled to the desorption zone third mix. first, second and first head streams.  The term feed stream refers to the stream through which the feedstock is transferred to the adsorbent.  The starting material contains one or more extractable components and one or more raffinate components.  The extractable component is a compound or type of compound that is most selectively absorbed by the adsorbent, while the raffinate component is a compound or type of compound that is less selectively absorbed.  Normal paraffins in the feed stream are extractable MELT components, while feed stream idoparaffins and most of the aromatic hydrocarbons are the raffinate components.  However, a small part of the original aromatic hydrocarbon adsor. Mounts on the surface of the particles of the adsorbent and poe.  It can be considered as an extractable component in the strict sense of the term.  The term extractable component refers to a more selectively adsorbable compound or type of compound that represents the target product of this process, for example, normal paraffins.  The term stripping material refers to a material capable of desorbing the extractable component.  The term first stripping material means a material capable of desorbing aromatics absorbed on the surface, but not capable of desorbing absorbed normal paraffins from an adsorbent, while the term second stripping material is desorbing material intended to desorb absorbed normal paraffins.  The term cleansing agent refers to a raffinate type compound accepted in the process for the first purpose of washing out the raffinate components from the non-selective empty volume of the absorbent.  The term desorbent stream or desorbent inlet stream designates the stream through which the desorbent material is fed to the adsorbent.  The term raffinate stream or raffinate output stream refers to the stream by which most of the raffinate components are removed from the adsorbent.  The composition of the raffinate stream may vary from 100% desorbing material to 100% raffinate components.  By the term extract extract, the output extract extract designates the flow, by which the extracted material, desorbed with desorbent material, is removed from the adsorbent.  The composition of the extract stream can also vary from 100% desorbing material to 100% of extracted components. I Although using the proposed invention it is possible to obtain high-purity normal paraffins with high recovery rates (90% or higher), it should be noted that as an extractable component It is absorbed by the adsorbent, so the rafinate component is not completely passed by the adsorbent.  Therefore, small amounts of raffinate components are present in the extract stream, and vice versa, small amounts of the extractable component are in the raffinate stream.  In addition, the flows of extract and raffinate additionally differ from each other and from the initial mixture by the ratio of the concentrations of the extracted component and the component of the raffinate characteristic of each particular stream.  The ratio of the concentration of adsorbed normal paraffins to the concentration of non-adsorbed isoparaffins will be the lowest in the raffinate stream, higher in the initial mixture and the highest in the extract stream.  Similarly, the concentration ratio. non-adsorbed isoparaffins and the concentration of adsorbed normal paraffins will be the highest in the raffinate stream, slightly lower and the lowest in the extract stream.  The term selective pore volume of an adsorbent is defined as the volume of an adsorbent that selectively adsorbs components extracted from a feed.  The term non-selective empty volume of an adsorbent is the volume of an adsorbent that does not selectively hold components extracted from the raw material.  This volume includes the adsorbent cavities containing inert areas and intermediate empty spaces between the particles of the adsorbent.  The selective pore volume and the non-selective empty volume are expressed in volumetric values and they are important for determining the exact fluid flow rates required for efficient working of the working area with a given amount of adsorbent.  When the adsorbent enters the working area, its non-selective empty volume together with the selective pore volume is filled with liquid in this area.  A non-selective empty volume is used in determining the amount of liquid that should be sent to the same zone in the opposite direction of the adsorbent to displace the liquid in the selective empty volume.  If the flow rate of the fluid directed into the zone is less than the flow rate of the non-selective empty volume of the adsorbent entering this zone, then a total increase in the fluid in the zone is observed. adsorbent.  Since this total increase is a liquid that is in the selective empty adsorbent in the selective empty volume, it is (increase, carry off} in many cases contains less selectively retained starting components.  In the definition. In these cases, the selective pore volume of the adsorbent may adsorb the raffinate material from the liquid surrounding the adsorbent, since in certain cases there is a competition between the extractable and raffinate materials during the adsorption in the selective pore volume.  If the adsorbent surrounds a relatively large amount of raffinate material with respect to the material being extracted, then the raffinate material becomes sufficiently competitive to be absorbed by the adsorbent.  The starting materials used in the proposed process are hydrocarbon fractions with a carbon number varying about 6 carbon atoms per molecule up to 30 carbon atoms per molecule.  The carbon number of hydrocarbon fractions can be significantly narrower, for example, from about three to ten carbon atoms.  The starting stream is the Qp-C C kerosene fraction) or C (gas oil fraction). . The feedstocks may contain normal paraffins, isoparaffins, and aromatic hydrocarbons in various concentrations, but may not contain olefins or contain them in small quantities. Depending on the type of raw material from which the hydrocarbon fraction is obtained, and on the range of the carbon number of this fraction, the concentration of normal paraffins can vary from 15 to 60 vol%, and the concentration of aromatic hydrocarbons can vary from 10 to 30 vol. % of the volume of raw materials.  More unusual can be raw material streams with aromatic hydrocarbon concentrations of 2–4 vol. %  Since the aromatic carbonic rocks of the raw material, like isoparaffins, do not enter the pores of the adsorbent, because the diameter of their cross section is too large, almost all of these aromatic hydrocarbons fall into the raffinate stream.  A small part and too adsorbed on the surface of the tea & particles of the adsorbent and necessarily falls as a contaminant into the extracted (normal paraffins) product.  Source aromatic hydrocarbons contain monocyclic aromatic hydrocarbons, for example, benzene or alkyl benzenes, indanes or alkyl indanes, and bicyclic aromatic hydrocarbons, including naphthalenes, biphenyls or acenaphthenes.  Aromatic impurities are characterized by the general formula - С H2j, j, where.  , as is customary in mass spectrometry, indicates a specific number, which, when substituted into an empirical formula, determines the difference between various complicated aromatic hydrocarbons.  Certain -jg and} amatical hydrocarbons are most strongly retained on the adsorbent.  Other types of aromatic hydrocarbons, such as jg or i Q, are also strongly adsorbed.  A certain purity of its substance preferably has a boiling point different from the boiling point of the raffinate component of the starting stream, so that it can be easily separated from the raffinate stream during distillation.  Thus, according to the inventive method, the cleansing agent is selected from high or low boiling homologues of isoparaffins or naphthenes of the feedstock.  An example of a suitable cleansing agent that is used in the isolation of normal paraffins from the C feedstock is isooctane, which is not absorbed by the adsorbent and is determined from the C-raffinate components by distillation.  The cleaning agent is fed at a rate equal to the space velocity of the empty space between the particles of the adsorbent passing a given point in the processing cycle at a given circulation rate, so that the adsorbent material is completely and continuously removed from the space between the particles of the adsorbent as it circulates. first of all raffinate ingredients.  The displaced raffinate components are combined into a liquid stream flowing through the adsorbent and ultimately removed from the circulating liquid phase as a raffinate stream, part of which is subsequently fed into the raffinate fractionation devices, where the raffinate components are removed.  The preferred rate of supply of the cleaning agent to the cleaning zone is equal to or greater than the rate of passage of the empty spaces between the particles of the adsorbent, which in each case depends on the size of the particles of the adsorbent, whether the moving bed or the stationary layer of particles is used in the process. tori.  The materials used in the proposed process are easily removed from the feed mixture.  Both the raffinate stream and the extract stream are recovered from the adsorbent in admixture with desorbing materials.  Without the separation of these stripping materials, the purity of the extraction of the components and the raffinate components, if desired, their extraction is not very high, and the desorption materials cannot be reused. in the process.  Therefore, the desorption materials have a boiling range that is different from that of the initial mixture, which allows the use of fractionation to separate the raffinate and extracted components and allows the desorption materials to be recovered so that they can be reused in the process.  The process may use one or two stripping materials.  It is not necessary to use the first stripping material, if it is necessary to obtain an extracted product containing a reduced concentration of the original aromatic hydrocarbon. When using the first stripping material, the concentration of the original aromatic hydrocarbons in the extracted product is reduced to less than 0.05 wt. % The first desorption materials used in the proposed process contain aromatic hydrocarbons having a boiling point different from that of the initial mixture to allow their separation by transfer.  It is also preferable that the first stripping material has a boiling point different from that of the cleaning agent in order to be able to separate them by distillation.  The first stripping materials are individual aromatic hydrocarbons, for example, benzene, toluene, xylene isomers and ethyl benzene or a mixture of aromatic hydrocarbons Cg.  In the example above, where normal paraffins are to be removed from the dg-C hydrocarbon feed stream, and isooctane is used as a cleaning agent, examples of suitable first desorbing materials are P. lol or ethylbenzene.  When a first desorbent is used in a mixture with a cleansing agent, the concentration of the first desorbing material of the mixture varies from about 5 to 100% of the total volume of the mixture.  A more preferred concentration range is between 15 to 40 vol. %  Since the goal of the first stripping material is to desorb only the adsorbed surfaces of the original aromatic hydrocarbons, it is also important that the first stripping material does not contain or contains a small amount of the second stripping material to avoid. desorption of paraffin paraffins.  In a preferred embodiment, the concentration of the second stripping material in the first stripping material should be less than 1.0 o6i. The second desorbing material contains any normal paraffin with a boiling point for personal separation from distillation of the initial see cm.  Normal pentane is used as the second desorbent, since it is easily separated from the raw material used in the process data sheet. The second desorbent material may be 100% normal paraffins, but may have a lower concentration of normal paraffins mixed with diluent Sisoparaffin or naphthene. .  When used in a mixture with a diluent, the concentration of normal paraffins is 40–80% by volume.  It is important that the second stripping material does not contain or contain a small amount of the first stripping material, so the presence of aromatic hydrocarbons prevents the desorption of normal paraffins from the second stripping material.  In a preferred embodiment, the concentration of the first desorbent in the second should be less than 0.1 vol. %  The solid adsorbents to be used in this case contain form-selective zeolites, known as molecular sieves.  The term selective in shape implies the ability of zeolites to separate a molecule according to their shape or size due to the fact that the pores of the zeolite have a fixed diameter in cross section.  Zeolites belong to the group of aluminum silicate crystals having a frame structure in which each tetrahedron of SiOi or AEO has common angles with another tetrahedron, and thus all silicon, aluminum and oxygen atoms are distributed in the structure.  These crystals have a chemical formula in which the ratio + Af /: / O / is 1: 2.  Of the different types of known zeolites, only those that have rigid carcass & are suitable as molecular sieves.  In personal molding, zeolite crystals contain water in the spaces of the skeleton.  With moderate heating, this water evaporates and creates open cavities of the same size, into which compounds penetrate, the maximum diameters of the molecules of which are slightly larger than the minimum diameters of the cavities. Pure zeolitic molecular sieves, especially synthetic molecular sieves, are obtained in the form of soft powder mass or small crystals. .  For use in industrial processes, these deolitic crystals are mixed with bonding materials, clay, silica, or other materials to form stronger, more resistant particles.  The adsorbents provided are zeolites with the same pore diameters of 5 A, for example, chabazite, or especially such as molecular sieves of the type 5 A, supplied.  Linda.  These latter sieves are typically in the form of an extrudate, pellets or in granular form and contain pure 5 A zeolite and a coherent material, such as clay.  The adsorbent used is in the form of particles of 20-40 mesh.
    The adsorbent is applied in the form of a dense compact fixed layer, which alternately contacts with
    the original mixture and desorbing materials. In the simplest device, the adsorbent is applied as a single fixed layer. In the other unit, a set of two or more fixed layers is used — with a corresponding switching in such a way that the initial mixture passes through one or several adsorption layers, while the desorbing material passes through one or several other layers from this set. The direction of flow of the initial mixture and desorbing materials through the adsorbent can be either bottom-up or top-down. Conventional devices for making contact liquid solid can also be used in a fixed bed.
    However, antirutine systems FJ with a moving layer or simulated countercurrent systems have a much greater separation efficiency than systems with a fixed layer of adsorbent, and therefore are preferred. In processes with a moving bed or with a simulated moving bed with a layer, adsorption and desorption proceed continuously, which allows both continuous production of extract and raffinate streams and continuous use of feedstock and lesorbent flows. One CS of the known variants of this process is similar to a countercurrent system with a moving bed. In such a system, there is a gradual movement of fluid through a plurality of passages downward of the adsorption chamber, which simulates upward movement of the adsorbent contained in the chamber. Typically, four lines operate at any time: the source flow line, the desorbent flow line, the raffinate flow line and the extract flow line. In accordance with this movement, as if simulating movement
    solid adsorbent upward, is the movement of fluid occupying the empty volume of the layer of adsorbent. To maintain countercurrent fluid contact downward, the adsorption chamber is equipped with a pump. Since the kaK fluid injection points are shifted through the cycle, the chamber circulation pump provides different zones that require different flow rates. A regulator with a nporpar / fiviHbiM control is established and adjusted for these costs.
    The injection points for active liquids effectively divide the adsorption chamber into separate zones, each of which has its own function. Three separate working zones must be used to carry out the process, although in some cases an optional fourth zone is used.
    The drawing shows a scheme that implements the proposed method.
    The adsorption zone 1 is determined by an adsorbent located between the inlet of the stream and the exit of the raffinate stream. In this zone, the feed is contacted with the adsorbent, the extractable component is adsorbed and the raffinate stream is withdrawn. Since the normal flow through zone 1 is directed from the flow of raw materials entering the zone to the flow of raffinate leaving the zone, the flow through the zone is considered to occur from top to bottom from the entrance of the flow of raw material to the exit of the flow of raffinate.
    Immediately (above the flow to zone 1) zone 2 is located. Purification zone 2 is defined as an adsorbent located between the exit of the extract stream and the inlet of the feed stream. The main operations occurring in zone 2 are the displacement from the non-selective empty volume of the adsorbent of any raffinate material falling into zone 2 when the adsorbent is moved to this zone, and the selective desorption of any raffinate material adsorbed in the pores of the selective volume of the adsorbent or adsorbed surface m particles of the adsorbent. These operations are carried out by passing a cleansing agent, desorbing material and part of the extract stream from zone 3 to zone 2, with the output border of zone 2 serving as the outlet of the extract stream. The flow of material in zone 2 is directed downwards from the outlet stream of the extract to the input stream of raw material.
    Above zone 2 is the desorption zone 3. The desorption zone 3 is defined as an adsorbent located between the desorbent inlet and the extract stream outlet. The purpose of the desorption zone 3 is to displace the normal paraffins adsorbed by the adsorbent during contact with zone 1 in the previous work cycle, the second material that is entering the zone. The flow of fluid in zone 3 occurs in the same direction as in zones 1 and 2.
    In some cases, the optional buffer zone 4 is used. This zone, defined as an adsorbent located between the GREAT raffinate stream and the incoming stream of desorbent, if present, is located above the stream 3. Zone 4 is used to preserve the amount of used at the stage of desorption of the sorbent, since part of the raffinate stream withdrawn from zone 1 enters zone 4 to replace the material inherent in this zone and to press it into the desorption zone. Zone 4 contains a sufficient amount of adsorbent, so that the raffinate present in the raffinate stream, passing from zone 1 and into zone 4, is prevented from falling into zone 3, thereby contaminating the extract stream that is removed from zone 3. In the case of x, when: the fourth working zone is not used, the raffinate flow, directed from zone 1 to zone 4, is carefully controlled so that the flow directly from zone 1 to zone 3 can be stopped, when in the raffinate flow passing from zone 1 to zone 3, there is a significant amount of valid material in order for t would not contaminate the effluent tract eq. Cyclic advancement of the inlet and outlet streams through the fixed adsorbent layer is carried out by means of a distribution system in which the valves on the pipelines act in series to move the inlet and outlet streams in such a way as to ensure opposite flow of the liquid relative to the solid adsorbent. Another way to work with providing a countercurrent solid adsorbent with respect to a liquid is to use a rotary disc valve, to which inlet and outlet flows and lines are connected, through which the feedstock flows, the withdrawn extract of the incoming desorbent, the recirculated raffinate product and the withdrawn the raffinate is advanced through the bed of adsorbent in the same direction. Both the collector device and the disc valve are known in the art. i In many cases, a working area contains a much larger amount of adsorbent than some other working area. For example, in some cases, the buffer zone contains the minimum amount of adsorbent compared to the amount of adsorbent required for the adsorption and purification zones. When a desorbent is used, which easily desorbs the extracted material from the adsorbent, a relatively small amount of adsorbent is needed in the desorption zone compared to the amount of adsorbent needed in the buffer zone, the cleaning zone, or in all of these zones. So, if it is not necessary that the adsorbent be in one column, then the scope of the invention includes the use of multiple chambers or a series of columns. It is of course necessary that all input or output streams are used at the same time and in many cases can be turned off, while others supply or discharge material. The device re-arranging the proposed method contains a series of individual layers connected by pipelines, after which the input or output pipelines are located, to which various input and output streams are attached, switched alternately and periodically for continuous operation. The connecting pipes are connected to transfer outlets. Pipelines, which under normal conditions do not work as a pipeline, through which the material enters the process or is removed from the process. I Although most of the adsorption separation processes take place both in the liquid and in the gas phase, it is preferable for this process. This is liquid phase operation due to lower temperature requirements and higher yields of the target normal paraffin achieved when working with the liquid phase. Adsorption can take place in a temperature range of 40-250 ° C and in a range of pressure variations from about atmospheric to about 35 atm to ensure liquid phase conditions. i Desorption can occur under the same conditions as absorption. A portion of the extract stream from zone 3. is sent to the first devices to fractionate the extract extract stream in order to separate it under appropriate conditions on the overhead, lateral and the bottom residue. The overhead contains a second stripping material and a cleansing agent, and, when using the first stripping material in the process, is less than O, T vol.% Of this first stripping material. The side product contains a cleansing agent, a lower concentration of the second desorbing material than the head one, and, when using the first desorbing material, the first desorbing material. The bottom residue is an extracted product or normal paraffins and contains almost no desorbing materials or cleaning agent. A part of the raffinate output stream is directed to the second devices for the fractionation of the withdrawn pot raffinate, where, under appropriate conditions, it is divided into head run, side run and bottom pogo. The head run contains second desorbing material, a cleansing agent, and, when used in the first desorption material, less than 0.1 vol% of this first desorption material. The side skirt contains a cleansing agent, a lower concentration of the second desorbent than the overhead, and, when using the first desorbing material, the first desorbing material. The bottom residue is a raffinate product (primarily isoparaffins and aromatic hydrocarbons) and, in the preferred embodiment, does not contain desorbing materials or a cleansing agent. The term does not contain indicates that the concentration of the desorbing material in both the extracted product and the raffinate product is less than 5% by volume, and in the preferred embodiment, less than 1% by volume. The two side straps are combined and sent to third fractionation devices, where the mixture is separated under appropriate conditions to produce a head fraction recirculated back to zone 3, and a bottom fraction recirculated back to zone 2. The head fraction contains the second desorption material and cleaning agent, and, when using the first stripping material, less than 0.1% by volume of the first stripping material. The bottom residue contains a cleansing agent, less than 1.0% by volume of the second desorbing material, and, when using the first desorbing material, the first desorbing material. By removing side straps from the first and second fractionation devices, each strand contains lower concentrations of the second stripping material, comparing the second stripping material with the concentrations of the second stripping material in the corresponding head straps in the energy of the third fractionation devices it is reduced compared with the same parameters without outputting side straps with the direction to the third fractionation devices The overhead of the first or second fractionation devices (of both fully and partially of each). The second stripping material is supplied relatively less per unit of time to the third fractionation devices, which makes it possible to reduce investment costs and operating costs for the third fractionation devices. The first, second, and third fractionation devices are distillation columns, the design and operation of which are well known in the separation technique. The size of the plants varies from pilot plant to industrial plant, and costs vary from a few cm per hour to many thousand liters per hour. The drawing shows four separate working zones and three separate fractionation devices, together with input and output streams and connecting pipelines. 1 to obtain the output stream of the extract and the output stream of the raffinate by separating normal paraffins from isoparaffins, use an adsorption zone 1, a purification zone 2, a desorption zone 3, and an optional buffer zone 4. To isolate the desorbing material and cleaning agent from the output streams of the extract and raffinate, to obtain target output streams of extract and raffinate are used. fractionation devices are 5 and b. To separate the desorbing material from the cleansing agent, fractionation devices 7 are used in the working area to reuse each of them. Four zones have stationary layers of solid adsorbent particles, but in other cases one or more chambers are connected in series. Each zone may be one chamber or a successive row of layers arranged one above the other in a column, forming zones. Thus, in some cases, each of the zones contains basically the same amount of adsorbent and has the same amount of adsorbent and the same basic physical dimensions, but in other cases some zones require a larger amount of adsorbent, h: other zones. The total flow of fluid through the zones occurs in the direction from top to bottom, but in some cases the zone operates in such a way that at a certain period of time the fluid in it flows in the direction opposite to the flow of the total fluid flow. In order to understand the processing steps occurring in different zones, the flow of the particles of the adsorbent is considered to occur from the bottom to the top. With normal countercurrent
    with a fixed bed of adsorbent, the material remains stationary, and separate adsorption, cleaning, desorption and buffer zones move through the adsorbent by switching various input and output streams in an indirect way to ensure the flow of fluid in the direction opposite to the adsorbent and for continuously obtaining extract streams and raffinate.
    In most cases, the input and output streams are switched in the direction of the fixed bed of desorbent at the same time and at the same distance along the length of the adsorbent bed. In other cases, it is necessary that between, two input and output streams, before switching them, the adsorbent performs the function of two
    or more zones. I
    The adsorption zone 1 is an adsorbent located between the inlet pipe 8 of the feedstock and the outlet pipe
    9 raffinate is connected to zone 1 by means of pipeline 10. Immediately, cleaning zone 2 is located above adsorption zone 1, and the input stream (pipeline) 8 serves as a common boundary between these zones. Purification zone 2 is an adsorbent located between the extract outlet stream 11 and the inlet stream.
    In the raw material. Immediately above the purification zone 2 is located the desorption zone 3, which is limited by the output stream 11 of the extract, as a common border with the purification zone 2. The desorption zone 3 is an adsorbent disposed between the outlet stream 11 of the extract and the inlet stream 12 of the desorbent. Immediately above the desorption zone 3, an optional buffer zone 4 is located, which is limited by the inlet stream 12 of the desorbent as a common border with the desorption zone 3 and is limited. the output stream 9 of the raffinate as a common border with zone 1 adsorption. The optional zone 4 is an adsorbent located between the inlet stream 12 of the desorbent and the outlet stream 9 of the raffinate.
    The end zones 1 and 4 are connected by pipes 13 and 10. The connecting pipes divert part of the liquid from zone 1 through line 10 to line 13 and zone 4 or zone 3, depending on whether an optional zone is used or not. thereby achieving a closed circulation of fluid. Pipelines 14-16 connect zones 1 and 2, zones 2 and 3, and zones 3 and 4, respectively, to allow a constant passage of fluid from one zone and through all the rest
    zone. In particular, the material coming out of the adsorption zone 1 through line 10 enters line 9 or part of it is withdrawn through line 13 to transfer eventually to the buffer zone 4. In the process of flow 9, the feedstock stream passes through the connecting pipe 14 and enters the adsorption zone 1. In some cases, part of it enters zone 2
     the cleaning line 14 of the liquid is mixed with the raw material entering the line .8 into the adsorption zone 1. The connecting pipe 15 allows in some cases to divert some of the liquid from the desorption zone 3 to the bypass line 11 and into the zone
    2 cleaning. Similarly, line 16 connects buffer zone 4 and zone
    Desorption and allows some of the liquid 20 leaving the buffer zone 4,
    mix with the input stream of contact material entering the process through the line 12 of the input stream of desorbent, and mixed with desorbent
    25 to submit to the zone 3 desorption. This makes it possible to reduce in the process the need for desorbent from external sources, namely, in the desorbent coming through line 12. On the line
    30 of the pipeline 13, a pump or other device for moving the liquid is installed so as to organize the flow of the liquid in the jB direction from the line 10 through line 13 and the buffer zone 4.
    Other pumps and valves located on the inlet and outlet pipelines and pipelines connecting the various zones and regulating the flow of the system are not shown. If necessary, they are installed for the installation and control of the flow rate of the liquid in the process by any specialist. Tom. Input streams coming into
    g various zones are connected to: high pressure sources or pumping devices, and the flows leaving the process are controlled by check valves
    : pressure. In cases where a bypass is not used around the pump, devices for unidirectional flow of liquid, such as non-return valves, are installed on the pipelines between different zones.
    The initial flow enters the process in zone 1 along line 8 and, since the general main flow direction of the fluid in zone 1 is downward, it moves along
    0 line 14 along with any material leaving zone 2 to zone 1.
    As the raw material enters zone 1, an equal volume of flow of raffinate material is displaced from it, leaving this zone through pipeline 10, Part or all. the rafknit gitt passing along the lin. 10, is removed from zone 1 via line 9, and any part of the flow that is not removable through line 13 enters 3 zone, 3 or zone 4, depending on whether the optional zone 4 is used in the process, the outgoing raffinate stream according to lines 8 are sent to fractionation devices 17, where the desorbing material and the purification are separated from the raffinate components.  The movement of the adsorbent in zone 1 is considered to be countercurrent (fluid motion in this zone.  The simulated flow of solids into and out of the adsorption zone occurs when the calls are switched during a portion of the input operation cycle.  I.  "The adsorbent entering zone 2 passes from zone 3 or 4, depending on whether the optional zone 4 is used or not in the process. If optional zone 4 is not used, then the adsorbent leaving zone 3 and entering zone 1 is mainly contains desorbent located in both non-selective empty spaces and selective empty spaces. In the case of using zone 4, a portion of the raffinate flow through line 13 is fed to zone 4 to displace the desorbing material from non-selective empty volumes of adsorbate particles located zone 4 via line 16 to zone 3.  Then it enters from the buffer zone 4 to the adsorption zone; 1, the adsorbent contains a large part of the desorbent, which was in the selective pore volume of the particles of the adsorbent extracting material, which is to be desorbed. in zone 1 (not shown).  Remove desorbing material. Of the selective pore volume, it is possible by additional contacting the adsorbent with a positive. o high-purity refined material before contacting the adsorbent with the incoming flow of raw materials in the upper part of the adsorption zone.  This feature is desirable in many systems, since it has been established that the absence of a desorbent in the adsorption zone improves the adsorbent's ability to selectively adsorb and retains the extractive component of the HY component with respect to the raffinate to ponent.  Moving upward through the adsorption zone 1 from its lower boundary towards the upper section of the fluid in this zone along the axis of the adsorption zone, the adsorbent absorbs extractive material from the incoming feed stream.  At the outlet from the adsorption zone, the adsorbent contains 5K and t eq with a t r and g and a ro rn a n t ma n t a r a n a l i n e which is the amount of refined material located in the selective pore volume of the adsorbent and some amount of raffinate material adsorbed on the surface of the adsorbent particles.  The material in the non-selective empty space of the adsorbent is a raffinate material with small portions of the material extracted from the raw material that is not adsorbed by the adsorbent.  Then this adsorbent is sent to the cleaning zone 2 at its boundary, indicated by a line (Pipeline / 8 feedstock input.  The adsorbent entering the cleaning zone 2 from the adsorption zone 1 contains a certain amount of raffinate material, located in the volume of the selective pores of the adsorbent, in a non-selective empty volume and adsorbed on the surfaces of the particles of the adsorbent.  The subsequent function of the cleaning zone 2 is THATING to remove the raffinate material from the selective pore volume of the adsorbent, the non-selective empty volume of the adsorbent, and from the surfaces of the particles of the adsorbent, so that the adsorbent leaving the cleaning zone through its upper boundary 11 contains very little raffinate material extracting product stream.  These functions are achieved in zone 2 in various ways.  Initially, part of the extract stream, a mixture of desorbent and extracted material enters zone 2 cleaned through line 15 and displaces all the raffinate material from the selective pore volume of the adsorbent and transports the displaced raffinate material and raffinate material from the non-selective pore volume of the adsorbent down to the convergent liquid stream. towards the exit line of the raffinate flow 9.  As can be seen from the drawing, the cleaning zone has a connection with line 7, through which a raffinate-type cleansing agent enters.  The cleaning agent itself supplements the detergent action of a portion of the extract stream entering zone 2 from zone 3 through line 15.  The cleansing agent can also allow the initial raffinate material to be removed from the adsorbent, reducing the amount of extract stream entering zone 2.  Reducing the amount of desorbing material contained as part of the extract stream entering zone 2 improves the ability of the adsorbent to absorb the last traces of the extracted material from the stream surrounding the adsorbent in the cleaning zone.  In addition, the cleansing agent, being a relatively non-adsorbable raffinate type material, does not increase the load on the adsorbent in zone 1 and therefore does not reduce the performance of the adsorbent with respect to fresh extractable material: entering the zone 1 through line 8, in the case of flow of the extract from zone 3 to zone 2 through line 15, however, the acceptable cost of the cleaning agent or extract stream is slightly removed with respect to, a small amount of raffinate material, part its adsorbent.  Although the bulk of the aromatic hydrocarbons entering the process comes out of the process as part of the raffinate effluent through line 9, a small portion of these aromatic hydrocarbons adsorb to the adsorbent particles in zone 1, passes with the adsorbent through zone 2 and desorbers into the desorbent . zone 3 appears as a contamination in the extract stream leaving the process through pipeline 11.  For this reason, in another embodiment of the invention, the first desorbing material in a mixture with a cleansing agent enters zone 2 through line 18.  When contacting in zone 2 of the adsorbent with the first desorbing material, the aromatic impurities adsorbed on the surface are desorbed from the particles of the adsorbent and are supplied using a cleaning agent and part of the extract stream entering zone 2 through line 15, downwards zone 2 in the direction of line 9, retraction the flow of raffinate.  The first desorption material is selected for the specific purpose of desorbing only aromatic impurities, but not. desorption of extracted normal paraffins.  Therefore, the adsorbent passing downstream from zone 2 to zone 3 contains normal paraffins in a selective pore volume and a greatly reduced concentration of pollutants of aromatic hydrocarbons on the surface of the particles of the adsorbent.  Although line 18 may be located anywhere along the adsorbent located in zone 2, from the highest point at line 11 of the extract stream to the lowest point at line 8 of the inlet of the original stream, it is preferable to place line 18 as close as possible to line 11 of the extract stream so that the cleansing substance or mixture of cleansing substance I.  and the first stripping material could. flow through most of the zone length and perform its respective functions.  Regulate the flow of fluid through the zone.  2 by adjusting the amount of material entering this zone through line 18, the material entering this zone from zone 3 along line 15, and the amount of material leaving and. from the highest part of zone 2 through line 14.  The adsorbent exiting from zone 2 enters the desorption zone 3 through the lower boundary of this zone - line 11 of the extract stream exit.  The operation of the desorption zone mainly consists in extracting normal paraffins from the adsorbent.  The extraction is carried out by contacting the adsorbent with a desorbing material capable of displacing normal paraffins from the volume of the selective pores of the adsorbent.  The adsorbent feed enters the desorption zone 3 at its upper boundary through pipelines 12 and 16. At least some of the desorbed normal paraffins leave the desorption zone 3 mixed with this desorbent material through the extract stream outlet line 11.  The extract effluent pipe 11 is then supplied to fractionation devices 5, where the paraffins are separated from the stripping material.  The adsorbent leaving the desorption zone 3 contains a desorbing material located both in the volume of the selective pores of the adsorbent and in the non-selective volume.  The adsorbent is then transferred to an optional; buffer zone 4, the entrance to it at its lower boundary - line 12 output stream of desorbing material.  Optional zone 4 in this process can be used as to conserve the amount; desorbent, and to prevent the extracted material from being contaminated with raffinate components.  When using work zone 4, a part of the raffinate outlet stream, not withdrawn via line 9, can be directed to zone 4 through pipelines 13 and 10 to displace the desorbing material from the non-selective empty volume of the adsorbent particles in zone 4 and to displace the desorbing material from optional zone 4 along lines 16 to zone 3.  Since the stripping material entering the process through line 12 returns to the Gyo pipeline, which connects optional zone 4 to desorption zone 3, desorption material displaced from the adsorbent in optional zone 4 tends to reduce the need for stripping material. -, le, entering the process through the pipeline 12.  The solid adsorbent, leaving zone 4 at its upper boundary — line 9 of the exit of the refiner stream 9 — contains mainly the desorbing material in the volume of the selective pores and the raffinate material with a non-selective empty volume of the adsorbent.  In the case of when the optional 4-zone is not used, a portion of the raffinate stream-from zone 1 is sent directly to zone 3, 3 of these cases, it is required that the material leaving zone 1 through line 10 and bypass line 9 does not contain raffinate material The initial raffinate material withdrawn from zone 1 contains a very high concentration of desorbing material and can be sent from line 13 and 10 to zone 3.  At this time, the flow of the raffinate effluent, which follows the process along line 9 -, may be blocked.  If passing through lines 13 and 10 to zone 3, the stream contains a noticeable amount. of the raffinate material, the flow to zone 3 via line 13 is stopped, and the output of the raffinate is then withdrawn along line 9.  Then the raffinate materials are output through line 9, external. . the source of the stripping material can feed zone 3 through lines 12 or 13, Inlet and weekend, lines 9, 8, 18 11 and 12 are filled with adequate flow during normal operation.  For continuous operation, it is necessary that separate input and output streams are different. In the same direction and in many cases at the same time.  By switching the input and output flow throughout the layer a. However, provided that the end zones (the adsorption zone 1 and the buffer zone 4 or the desorption zone 3; they have a connecting pipeline, separate operations can be carried out continuously in different zones.  When the described zones vary in increments of quantities of flows flowing through the stationary layer of the adsorbent, the adsorbent contacts the next after. Convenience: adsorption. zone, - the area of eyeglasses. , the desorption zone and the buffer zone, respectively. At least a part of the extra-current input and current. Kta on line 11 enters the fractionation devices 5, where under appropriate conditions. It is processed to produce a head wrap, discharged along lines 19, a side wrap, wedge. Limogogue on line 20 and bottoms produced from the line 17 “At least part of the output. The bottom flow of the raffinate is fed through line 9. to fractionation devices b, where it is processed. ; under appropriate conditions, to obtain a head wrap, discharged through line 21, a side wrap, discharged through line 22 and a bottom cube, discharged along line 23.  The side straps discharged along lines 20 and 22 are combined and the mixture is sent via line 24 to fractionation devices 7.  The fractionation devices 7 operate under appropriate conditions for the production of a head crown discharged through line 25 and a cube crown discharged. through line 18, the bottom fraction from fractionation devices 7 is recycled back to zone 2 via line 18, the head fraction from fractionation devices 7 withdrawn along line 25 is combined with the leading epaulet from fractionation devices 5 withdrawn along line 19, and.  the mixture of two head straps is withdrawn via line 26. This mixture is in turn combined with the head straps from fractionation devices 6, and the mixture of all three head straps is withdrawn along line 12 and returned back to zone 3 as an inlet de-orbent stream.  For the initial filling of the system or to compensate for losses, a first stripping material, a second stripping material and a cleaning agent, respectively, can be added to lines from the external sources via lines 27, 28 and 29.  Example.  An apparatus for isolating normal paraffin from a hydrogen treated kerosene fraction.  The first adsorption section of this process.  In this section, a simulated countercurrent fixed bed contacting system and a ball valve distribution device are used to achieve continuous contact of the feed stream and desorbing materials with the adsorbent in certain zones II of continuous extraction of the extract and raffinate streams from the adsorbent maintained in certain zones.  The quality of the adsorbent uses 100 tons of molecular sieves 5 A, Lin. Each loaded layer has two serially connected chambers, each divided into 12 equal layers. Each layer has a transfer valve to which a transfer line is attached, through which the material can pass into or out of the layer in accordance with the preferred cycle of operations. Time cycle for ball valve (or the time of one cycle of operation / is 5 minutes.  A system of four zones is used: zones 1, 2 and 3 each contain 7 layers of adsorbent, and zone 4 contains 3 layers of adsorbent.  The operating temperature and pressure are 177 and 24.6 ati, respectively, in the adsorption chamber, adsorption and desorption are carried out in the liquid phase.  To obtain the extracted product C of normal paraffins containing less than 0.005 weight. % of the original aromatic hydrocarbons, use two desorber materials.  The first stripping material was a mixture of Cg aromatic hydrocarbons, entering zone 2 mixed with isooctane as a cleaning agent.  The mixture entering zone 2 contains 70 vol. % isooctane and 30 vol. % Cg of aromatic hydrocarbons with a maximum amount of second desorbing material about 1 vol. %  At steady-state operation, the flow rate of this mixture is 316 barrels per daily flow (500 m / s. The second desorbing material is normal pentane.  Zone 3 receives a mixture of 60 vol. % normal pentane, 40% isooctane as a diluent, and the most out of. 0.1 vol. % of the first d sorbent material.  When installed, the flow rate of this mixture is 7154 barrels per day (from m / day).  The costs of other flows during steady-state operation are: the initial flow to zone 1 900 of MVcyx, the flow of extract from zone 3 2740 MVcyT and the flow of raffinate withdrawn from zone 1 1310 MVcyT.  I Operation of fractionation devices and devices for recirculating the sorbent process.  1150 of the output stream of the extract is sent to the fractionation column of the extract, in which 610 of the extracts are obtained, 342 of the extracts and 214 canine residue or the target extract.  The composition of the head shoulder includes 67.0 vol. % normal pentata and 33 mol. % isooctane; the composition of the side product is 13.0 mol. % of normal foam, 73.6 mol.  % isooctane and 13, 4 mol.  % of aromatic hydrocarbons Cg, and the composition of the target extract includes about 99 mol. % normal paraffins.  The extraction column has an outer diameter of 1800 mm and contains 50 valve plates located 600 mm from each other, with the extracted stream being fed to the 34 plate and the side stream taken from the plate 20.  Working pressures are 1.4; 1.55 and 1.83 ati, and the working temperatures are 101, 122 and, at the top of the column, there is a side-by-side selection plate and at the bottom of the column, respectively.  The output of raLinat in the amount of 8312 barrels / day (1150 m / day is sent to a fractionation column in which 2516 barrels are obtained.  leu / day (345 m / day of the head raffinate shoulder strap, 1438 barrels / day (197 m VcyT of the side raffinate shoulder strap and 4358 barrels / day boo m / day} of the cubic raffinate residue.  Head shoulder strap consists of 66.7 mol. % of normal pentane and 33.3 mol. % isooctane; lateral shoulder strap contains 6.9 mol. % of normal pentane, 42.9 mol. % isooctane and 50, 2 mol. % of aromatic hydrocarbons Cg and the bottom residue contains 1.2 mol.  normal paraffins, 29.2 mol. % naphthenes, 45.0 mol. % of the original isoparaffins and 24.6 mol. % of the original aromatic hydrocarbons.  The raffinate column has an outer diameter of 2200 mm and contains 60 valve plates located 600 mm from each other, with the raffinate stream entering the plate 38, and the side stream is taken from the plate 20.  Working pressures are 1.4; 1.55 and 1.9 ati, and the working temperatures are about 101, 138 both at the top of the column, on the side-by-side selection plate and in the cube, respectively.  The side stream of the extraction column and the side stream from the raffinate column together with 413 barrels / day 57 MVcyT) a mixture of isooctane and Cg aromatic hydrocarbons used as a ball valve sealer, in a mixture sent to a desorbent fractionation column, in which 802 barrels / day are obtained (111 of the split overhead and 3164 barrels / day (436) of the split bottoms.  The head shoulder strap consists of 44.6 mol. % of normal pentane and 45.4 mol. % isooctane, while the VAT residue contained 62.2 mol. % isooctane and 37.8 mol. % aromatic hydrocarbon Cg.  The split desorbent column has an outer diameter of 100 mm and contains 25 valve plates located 600 mm apart from each other with a power supply of 16 plates.  The barge pressure is about 1.76 and 2.04 bpm, and the operating temperatures are about 119 and 15 bps for the top and bottom of the column, respectively.  The bottoms from the desorbent cleavage column are recycled back to zone 2 of the adsorption section, and the head cake from the desorbent splitting column, together with the head cake from the extraction column and the head cake from the raffinate column, are returned to zone 3 of the adsorption section.  The method of separating normal paraffinic hydrocarbons from a mixture containing isoparaffinic hydrocarbons, by directing the feedstock in the liquid phase to a column filled with an adsorbent selective for normal paraffinic hydrocarbons, and having at least three functional zones arranged in series and mutually connected , including end zones, providing a continuous cyclic flow in one direction in the following order: the adsorption zone, located between the incoming flow of raw materials at the upper and the output (by the flow of the obtained raffinate at the lower boundary; the purification zone located above the adsorption zone, located between the output flow of the obtained extract at the upper boundary and the input flow of the raw material at the lower boundary, and having an incoming flow of purifying an agent located above the incoming feed stream; a desorption zone located above the purification zone is located between the incoming sorbent desiccant stream at the upper boundary and the extract effluent stream at the lower boundary, feeding the purification zone into the purification zone exists a raffinate-type adsorption zone -. feedstock with the process of adsorption of normal paraffin hydrocarbons at a temperature of 40-25 ° C and a pressure of 1-35 atm and output of a raffinate stream containing isoparaffin hydrocarbons, a cleansing agent and desorben to the desorption zone -. desorbing with the process of desorption of normal paraffinic hydrocarbons at a temperature of 40-250 0 and a pressure of 1-35a and the withdrawal of noTOKs extract containing normal paraffinic hydrocarbons, a cleansing agent and desorbent, followed by the flow of the extract into the first fractionation devices to produce the first head a stream containing a mixture of a cleansing agent and a desorbent, and a first bottom fraction containing normal paraffin hydrocarbons, a raffinate stream to the second fractionation devices with the obtained Separating a second head stream consisting of a mixture of a cleansing agent and a desorbent, and a second bottoms residue containing isoparaffin hydrocarbons them in the desorption and purification zones with the process of separation with periodic displacement of functional zones in the direction of the liquid flow inside the column through the mass of adsorb The extract and continuous flows of the obtained extract and raffinate, characterized in that, in order to reduce energy costs, the separation in the first and second fractionation devices is carried out with the selection of side cuts withdrawn above the feed point of the raw fractionation devices, with a mixture of side cuts at the third fractionation devices and for recycling to de-zone.  Sorption directs the mixture of the third, second, and first head streams.  Sources of information taken into account during the examination 1. US Patent No. 3753896, cl.  208-310, published.  1973.  2 U.S. Patent No. 3,715,409, Cl.  260-674 SA, publ.  1973 (prototype).  L /
    权利要求:
    Claims (1)
    [1]
    Formula A Invented
    A method of separating normal paraffin hydrocarbons from a mixture containing 'isoparaffin hydrocarbons, by directing the feedstock in a liquid phase to a column filled with an adsorbent selective to normal paraffinic hydrocarbons and having at least' three functional zones arranged in series and mutually connected, including end zones providing a continuous cyclic flow in one direction in the following order: adsorption zone located between the incoming feed stream at the upper boundaries and the effluent obtained raffinate at the lower end, 'treatment zone located above the zone of adsorption, located between the effluent obtained extract at the upper limit and the incoming feedstock stream at the lower end, and having inlet flow cleaning agent disposed above the incoming feedstock flow; a desorption zone located above the purification zone, located between the inlet stream of the desorbent at the upper boundary and the outlet stream of the extract at the lower boundary, with the raffinate-type cleansing agent being fed into the purification zone, into the adsorption zone of the feedstock using an adsorption process for normal paraffin hydrocarbons at a temperature 40-250 ° C and a pressure of 1–35 atm and a stream of raffinate containing isoparaffin hydrocarbons, a cleaning agent and a desorbent is withdrawn to the desorption zone — a desorbent with a normal desorption process paraffin hydrocarbons at a temperature of 40-250 ° C and a pressure of 1-35 atm and the output stream of the extract containing normal paraffin hydrocarbons, a cleaning agent and desorbent, followed by directing the extract stream to the first fractionation devices to obtain the first head stream containing a cleaning mixture substances and desorbent, and the first bottoms fraction containing normal paraffinic hydrocarbons, the raffinate stream into the second fractionation device to obtain a second head stream, consisting of and a cleaning agent and a desorbent, and a second bottoms residue containing isoparaffin hydrocarbons, separating a mixture of a cleaning agent and a desorbent in third fractionation devices to obtain a third overhead stream of the desorbent and a third bottoms stream — a cleaning agent — and recirculating them to the desorption and purification zones using a process allocation during periodic displacement of the functional zones in the direction of the liquid flow inside the column through the mass of adsorbent and continuous flows of the obtained extract and Finate, characterized in that, in order to reduce energy consumption, the separation in the first and second fractionating devices is carried out with the selection of side straps diverted above the feed point of the fractionating devices, with the mixture of side straps being fed to the third fractionating devices and the mixture is recycled to the desorption zone third, second and first head streams.
    类似技术:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/633,183|US4006197A|1975-11-19|1975-11-19|Process for separating normal paraffins|
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