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    • 专利摘要:
    A process for separating raw soap from black liquor, using a wash liquor which is either pH-adjusted residual liquid from a tall oil-producing process step (180) or a pH-controlled aqueous solution of ash, wherein black liquor-containing soap is mixed with said wash liquor, and wherein waste soap is separated. the resulting mixture. The method comprises the steps of a) performing a first coarse separation (120,130) of raw soap from said black liquor to form a first raw soap fraction; b) mixing (140) the first raw soap fraction with wash liquor to form a first diluted fraction; and c) performing a separation (150) of the first diluted fraction, using a first centrifugal separator-type centrifugal separator, so that a second crude number soap fraction is obtained. The second raw soap fraction contains lower levels of black liquor than the first raw soap fraction. The invention also relates to a system. Application text 2014-12-10 140030EN
    公开号:SE1451515A1
    申请号:SE1451515
    申请日:2014-12-10
    公开日:2016-06-11
    发明作者:Göran Hofstedt Anders
    申请人:Göran Hofstedt Anders；
    IPC主号:
    专利说明:

    Procedure and plant for washing raw pine soapThe present invention relates to a method and asystems for washing raw pine soap.
    In pulp production with the aid of the sulphate process, crude pine soap is formed, which is readily mixed in the so-called black liquor. It is desirable to separate the crude pine soap, pretreatment in later process steps with acid, usually sulfuric acid, to produce tall oil, which is a raw material with manyapplications.
    In order to achieve good results in the production of tall oil from crude pine soap, it is desirable that the incoming crude pine soap be relatively clean, with as low proportions of black liquor as possible, since the black liquor contains dissolved lignin which precipitateswhen the raw soap, through. acidification, split into tall oil.
    In addition, black liquor contains calcium, in the form of, among other thingscalcium carbonate, as well as cellulose fibers. It is therefore desirable that the relatively pure crude pine soap contains as low proportions of black liquor as possible. Said precipitated lignin gives rise to sludge which is expensive and cumbersome to handle, and calcium contributes to answering precipitates on the equipment used.
    In order to separate black liquor, and thereby lignin and calcium, from the crude pine soap, it has been proposed, in US 8,419,897 B2, to use the residual liquid from the acid treatment of the crude pine soap, which residual liquid has first been treated with sodium hydroxide to form a solution with a pH value. between 10-14. This alkaline residual liquid is mixed with the contaminated raw soap,after the soap is separated out of the resulting mixture.
    Application text 2014-12-10 140030ENAdmittedly, such a procedure provides better separationblack liquor, and thus lignin and calcium, in the pastprior art, but takes a long time, requires bulky equipment and produces a soap that still contains significant proportions of black liquor and other contaminants, such as precipitated lignin, such as precipitated lignin. The present invention solves these problems.
    Thus, the invention relates to a process for purifying crude pine soap from black liquor, in which a wash liquor is used, which wash liquor either harrows from a tall oil-producing process step in which crude pine soap is treated with acid allowed to form tall oil, the residual liquid being an acidic residual water phase process steps which are pH-adjusted, or alternatively that the wash liquor consists of a pH-controlled aqueous solution of ash, whereby black liquor-containing crude pine soap is mixed with said wash liquor, and wherein crude pine soap is then separated from the resulting mixture, the process may comprise steps a ) performing a first coarse separation of crude tall soap from said black liquor so as to form a first rough soap soap fraction; b) mixing the first crude pine soap fraction with wash liquor to form a first diluted fraction;and c) performing a separation of the first dilutedfraction, by means of a purifier-type first centrifugal separator, so that a second crude soap fraction is obtained, the second crude soap fraction containing lower levels ofblack liquor on the first crude pine soap fraction.
    In addition, the invention relates to a system according totent requirement 15.
    Application text 2014-12-10 140030ENThe invention will now be described in detail, with reference to exemplary embodiments of the invention and the accompanying drawings, in which: Figure 1 is a general view of a system according to the present invention for carrying out a method according to the invention;Figure 2 is a schematic diagram of an open centrifugal separator of purifier; andFigure 3 is a schematic diagram of a hermetic centrifugal separator.purifier type rator.
    Figure 1 shows a system 100 according to the present invention for use in a method according to the invention. Specifically, the system 100 is useful in a process of the invention for washing out, or purifying, crude soap from black liquor, in other words for purifying a black liquor-containing mixture of crude soap so that the content of black liquor in the purified crude soap is reduced after purification. In addition, the system 100 and method of the invention provide a crude pine soap with low levels of other impurities, such as, for example, cellulose fibers andcalcium carbonate.
    In Figure 1, 110 denotes a conventional cooking step per sein a pulp production process according to the sulphate method,which step 110 as. residual product provides relativelylarge volumes of black liquor. This black liquor is passed to a separation stage 120, which can preferably, but not necessarily, be used for the present purpose and the purpose of which is to carry out an initial separation of black liquor from crude pine soap. It is preferred that,as shown in Figure 1, the separation stepconsists of a gravimetric separation tank, in which raw soap is due to the density difference in relation to black liquorallowed to float to the surface so that a relatively concentratedApplication text 2014-12-10 140030ENRaw tall soap fraction 122 is formed liquid on top of a fraction ofrelatively concentrated black liquor 121. The black liquor fraction 121is passed on to a subsequent process step, such as a combination of a per se conventional evaporation plant 101 and a subsequent, conventional recovery boiler 102. The flue gases of the recovery boiler 102 are transferred to a per se conventional electric filter 103, arranged in the flue gas stream from the recovery boiler 102 and separating ash particles from the flue gases . The gaseous partsof the flue gases depart in a flood 103a, and the separated, solidand the particulate ash is passed on to a dissolving device 104, such as a tank, where ash particles are dissolved in water to form an aqueous solution of such ash. Not lost material departs in a flood 104a. The water discharge of ash from the recovery boiler102 is led,according to one aspect of the invention, to a step 181(see below).
    Thus, the system 100 may, but need not, include separators.step 120. In that case, the separation step 120 is usedIt is preferred that the crude soap fraction 122 be added to, andfurther iq an initial centrifugal separation step130. The step 130 comprises a centrifugal separator arrangedseparating the fed black liquor mixed crude pine soap to form a separated black liquor fraction, which is returned torose 120; a fraction containing solid material, includingfibers and other contaminants which are carried to a subsequent treatment step, such as the recovery boiler 102; and a raw numbersoap fraction, which is passed on to step 140 (see below). The solid fraction is removed via a per se conventional and ice step 130 launching device 131 for solid particles.
    Figure 1 also illustrates a separation step 135, as an alternative to the separation step 130, in the form of aline consisting of one or more tanks, which are alsoApplication text 2014-12-10 140030ENarranged to separate the fed black liquor mixed raw pine soap so that corresponding fractions are formed as with the aid of step 130.
    The steps 120 and 130 illustrated in Figure 1, alternatively 120and 135, in combination with each other, constitute a step forperform a first coarse separation according to the invention. According to various embodiments of the invention, the coarse separation step may, but need not, comprise a gravimetric tank 120. Thus, the first coarse separation step may comprise a separation of a crude number soap fraction by means of a centrifugal separator, alternatively a separation of a crude number separation separation in tank 120, and a subsequent initial centrifugation step 130, alternatively a separation of a crude number soap fraction by means of gravimetric separation into several successive tanks 120, 135. In that case only gravimetric separation is used, it is also preferred to separate solid, contained in black liquor.particles in this way.
    Conventionally used for separation so-called centrifugalHigh Speed Separators (HSS)in which a separation chamber rotates, preferably withat least 1000 revolutions per minute, such as at least 3000 revolutions per minute, preferably at least 5000 revolutions per minute, thus creating a radial centrifugal force acting on the material present in the chamber. A relatively lighter phase is thus pressed. the center of rotation of the counter-chamber, while a relatively heavier phase is pressed outwards towards the periphery of the chamber. To increase the separation efficiency, stacks of stacked conical separation plates are used in the chamber. A separator of this type is describedtear down, for example, EP2664385 A1.
    There are different types of centrifugal separators.
    Application text 2014-12-10 140030ENIn so-called open separators, the phase mixture is fed in throughan inlet, separated and delivered at different outlets. A typeof such open separators deliver the phases at respective outlets at atmospheric pressure, which generally requires externalpumps for further removal of the phase in question.
    With the help of so-called shell disks, acting as centripetalpumps, the separated phases can instead be delivered at thespecific outlet with a certain pressure. In a separator of thistype, as described, for example, in SE534386 C2, the spruce level inchamber, that is to say the horizontal distance from theThe center between the separated phases is adjusted to change the width of so-calledgives, by"Gravity discs" or "level discs", hereinafter referred to as "level discs". With such leveling, the radial level of the heavier phase, which exerts a pressure against the later phase towards the center of rotation, can thus be adjusted.
    In such a separator, the heavier phase is pumped out via a shell disc device with its edge radially outside a corresponding shell disc which pumps out of the lighter phase. Because the shell discs are fixedarranged, and thus does not rotate with the chamber, there is a risk of leakage from the heavier phase to the lighter phase, especially if the pressure in the heavier phase is high.
    A so-called hermetic separator, or hermetically sealed separatorparator, on the other hand, is designed so that no free passageInstead, the initial pressure is created by pumping the mixture in the separator at an overpressure, which overpressure is also used to create a back pressure by means of so-called counter-pressures.pressure valves arranged on the outgoing phases, whichApplication text 2014-12-10 140030ENtiler regulates the team for the spruce level in the house. Such ametic separator is described, for example, in SE0950840 A1. Further distinguishing features of a hermetic separator are that the separator during operation is completely filled with added mixture and separated phases, and that no air is then present in the separator; and that a pressure applied at the inlet is propagatedto a corresponding pressure at the outlet.
    There are also different types of separators depending on which phase is to be primarily purified from the other. For this purpose, the through hole in said stack of separation plates is used at a certain distance from the center of rotation. This means that the two phases have different distances to travel in a radial direction before being collected. For maximum purification of the light phase, a so-called purifier is used, where the holes are arranged relatively far from the center of rotation. For maximum purification of the heavy phase, a so-called concentrator is used, where the holes are arranged.relatively near the center of rotation.
    Such a purifier type centrifugal separator is illustrated inFigure 2, in the form of a per se conventional, open centrifugalseparator 200, comprising a central inlet 211 for the mixture through which the mixture is introduced into the chamber 210 for separation therein and discharge via respective outlets 212 for a slurry phase 241 and 213 for a heavy phase 242. The two phases 214, 242 and the mixture of they are marked with different types of dashed lines in Figures 2 and 3.
    The chamber 210 is rotated, preferably at a rotational speedof at least 1000, more preferably at least 3000, more preferably at leastabout 5000, revolutions per minute by means of a drive mechanism acting on a shaft 220. A stack of a plurality of separation plates230 is used to increase the efficiency of the separation, onone in itself conventionally set. The light phase 241 is pressedApplication text 2014-12-10 140030ENradially inwards, and pumped out via a stationary centerripetal pump 216 (hidden in Figure 2). In the corresponding way is pressedthe heavy phase 242 radially outwards, and is pumped out via a stationary centripetal pump 217 (also concealed in Figure 2). To regulate the radial, horizontal distance between the rotation center of the chamber 210 and the spruce layer 243 between the lath 241and. the heavy 242 fraction is used respectivelyadjustable levels 214, 215 in a conventional manner.
    The centripetal pumps 216, 217, provide a certain overpressure of the separated phases 241 and 242 discharged from the outlets 212 and 213.
    The separating plates 230 comprise through holes 231, preferably arranged opposite each other so that a through, substantially vertical, channel is formed through the stack. The through holes 231 are arranged at a relatively large radial distance from the center of rotation of the chamber which causes the phase 241 discharged through the outlet 212 to be relatively clean, preferably cleaner than the heavy phase 242 whichdischarged through the outlet 213.
    To illustrate the difference between a purifier-type centrifugal separator and a concentrator-type centrifugal separator, which later, in contrast to the purifier-type separator illustrated in Figure 2, provides a separation to which the heavy phase is purified to a relatively greater extent than the late phase, possible radially low layer L, relatively small radial distance from the center of rotation, for the holes 231, which low L would have been usable if separated.the rator 200 had been of the concentrator type.
    Application text 2014-12-10 140030ENThe light phase will thus, due to the use of the pump 216,212.to be delivered with a certain overpressure at the outletIt will be appreciated that in the present process the light phase consists mainly of crude pine soap with some admixture of black liquor and wash liquor, while the heavy phase is mainly also of mixture of black liquor with some, very small, admixture of crude pine soap, and on the other hand wash liquor. impurities 250 in solid form, including fibrous sludge, in the mixture of black liquor and crude pine soap to be separated. These solid contaminants are separated out by the conventional ejection device 251, which is arranged to intermittently separate solid phase contaminants 250 which have accumulated in the separator 200 during operation, such as at regular intervals. The solid particles 250 may also comprise calcium compounds, such as calcium carbonate. Figure 3 corresponds to Figure 2, but shows a hermetic centrifugal separator 300 of the purifier type. The separator 300 comprises, like the separator 200, a stack of separation plates 330 with holes 331 which form a substantially vertical, continuous channel through the stack 330. The mixture is supplied via an inlet which on the correspondingrather311 arranged by a rotating shaft 320, set which for the separator 200 is driven by at least 1000, more preferably at least 5000, andat least 3000 rpm,thus also rotating the chamber 310 at this speed.
    The radial horizontal distance from the center of rotation of the chamber 310 of a spruce layer 343 between the separated slat phase 341 and the separated heavy phase 342 is controlled byto regulate different back pressures on outgoing phases, which are made possibleApplication text 2014-12-10 140030ENof an overpressure by means of which the mixture is supplied to the inlet 311. Via an outlet 312 the light phase is supplied with certain impurities of the heavy phase; via an outlet 313 the heavy phase is supplied with certain impurities of that slat phase. It is possible to use a co-rotating impeller in the outlets for both or either phase, which means that it is possible to achieve a selected pressure of the respective outflow phase. However, it is not preferable to use a pump arranged in such a flow, especially not for the heavy phase, since a high pressure is uniformly upstream of the separator to provide sufficient pressure to extrude the lat phase. Since the holes 331 are arranged relatively far from the center of rotation, in a manner similar to that described above for the separator 200, the light phase 341 supplied via the outlet 312 will be relatively clean, preferably cleaner.to the heavy phase 342 which is delivered via the outlet 313.
    A difference between the separators 200 and 300 is that of the phases341, 342 delivered from the outlets 312, 313 may have a larger oneoverpressure at the outlets 312, 313 of the phases 241, 242 suppliedfrom the outlets 212, 213, since the mixture is alreadyis at an overpressure via the inlet 311. In order to achieve this overpressure, a per se conventional pump can be used. In addition, a greater back pressure can be applied to the heavy phase 342 than is possible for the heavy phase 242, since too high a back pressure on the phase 242 risks causing leakage from the phase 242 to the light phase 241 in the separator 200, or ejection out of the separator by the space between the rotating body and the inlet pipes.
    For all of these separators 200, 300 described herein, it is preferred that the radial distance of the spruce layer 243, 343 from the center of rotation be adjusted to be approximately within thelen 231, 331.
    Application text 2014-12-10 140030ENThe distances between the separation plates 230, 330 are preferably a maximum of 3 mm, preferably between about 0.5 and 2 mm. It is preferred that the centrifugal separator 130, in Figure 1, comprises separation plates as described above, which are thus operative to separate a relatively heavier phase from a relatively lighter phase, as well as working at least1000, preferably at least 3000, preferably at least 5000 revolutions perminute. The same applies to the separators in steps 150 and 170(see below).
    In the present system 100 and method for separating raw pine soap from black liquor, a washing liquid of one of two possibleleague types.
    According to a first alternative, the washing liquid may be a residual liquid originating180.from a tall oil producing process step In process step 180, crude pine soap is treated with acid, such assulfuric acid, to form tall oil. Such process steps are icy conventional and are used for the production of pine oil from a raw material consisting of crude pine soap, by adding acid to the crude pine soap, whereby the crude pine soap is converted into pine oil and acid water (residual acid). It is preferred that step 180 be provided within the same facility as the rest of the system 100.
    After the conversion, an acidic solution remains, which is sometimes called residual acid, and which thus consists of an acidic residual liquid phase,180.preferably an aqueous solution, from the process stepThis residual acid is pH-adjusted in a step 181, to a basicThe pH value is preferably between 10 and 14,preferably between 11 and 12. The pH adjustment can take place, for exampleby adding sodium hydroxide NaOH, alternatively white liquor.
    Application text 2014-12-10 140030EN12The pH-regulating residual acid, which is now otherwise alkaline, is calledherein "residual liquid", and is used according to the invention, in pure formulas in recycled form after a first use in washing steps (see below), for washing raw soap from the contentsblack liquor.
    Another alternative according to the invention is a washing solution using a liquid solution of the above-mentioned box from the soda ashtray 102, such as after extraction in the electric filter 103 and dissolved in the tank 104. Preferably, the device 104 is a system for continuous ash solution with the help of washing liquid, to the step 181. It is preferred that the ash solution here be a dry sub-stencil content ts äv äskä om. at least 8%, more preferably 8% -23%,preferably 13% -17%, preferably about 15%. A dry matter content of at least 8% means that essentially no counting oil soap is dissolved in the ice solution when it is used as washing liquid. The ash solution pH is preferably adjusted in a corresponding manner as residual liquid, such as with NaOH or white liquor.and 14, preferably between 11 and 12.to a pH value also between 10In the following, the term "washing liquid" is used for the purpose of referring to either residual liquid or ash discharge according to the adjective. In some cases, it is also conceivable that "washing liquid" is used as a blender, as well as residual liquid and ash discharge in various processes.portions.
    That råtällsåpän is "washed" here means that it is blinded with onedetergent (such as washing liquid), then raw soapis blown out of the glare, which causes a washable friction ion which contains a smaller proportion of black liquor than water which is trapped with the friction before the washing step. According to the inventionThe mixture is thus blended with black liquor-containing raw soapApplication text 2014-12-10 140030EN13said wash liquor, after which crude pine soap is separated from thethe starving mixture.
    A washbasin as in one (or more) previous washing stepsused as wash liquor also constitute, in the terminus of the invention,lodging, washing, even if. it may include larger orless polluting proportions of black liquor from said earlier washing steps.as described above, a first coarse separatorring 120, 130 of raw soap from the contaminant contained in the raw soap, so that a first raw soap fraction is formed.
    This first crude soap fraction is taken to a first mixing device 140, in which the first crude soap fraction is mixed.das with wash water so that a first diluted fraction is formed.
    The first diluted fraction is passed to a first centrifugal separation step 150, comprising a centrifugal separator arranged to perform a separation of the first diluted fraction ion, so that a second crude soap fraction is obtained. The second raw soap fraction contains a lower content of black liquor than the first raw soap fraction, and is thus purified in proportionto the first crude number soap fraction.
    According to a preferred embodiment, the first centrifugal separator is of the hermetically sealed type, preferably of the type illustrated in Figure 3 and as described above. Thus, sufficiently high inlet pressure is used for the first diluted fraction so that a very good separation can be achieved by the light fraction (that is, raw pine soap with small impurities of black liquor and wash liquor).(it wantsand the heavythe faction saga wash water with contaminants ofApplication text 2014-12-10 140030EN14black liquor and only small contaminants of raw pine soap). It ispreferably this inlet pressure, for the centrifugal separator 150 and / or 170, is an overpressure of at least 5 bar, preferably 10 bar. This pressure can be achieved on the edge itself, as aided by a pump arranged upstream of the respective centrifuges.fugalseparator 150, 170.
    The present inventors have surprisingly discovered that it is possible to use a washing with the aid of such a centrifugal separator 150 to obtain very good purification results of the crude pine soap, when the pH-regulated residual acid from step 180 is used.water, or alternatively pH-regulated. ash solution from step 104.
    This purification process is also much simpler and fasterthan that described in US 8,419,897 B2.
    The separated, black liquor-containing, heavy phase is brought to a singlesubsequent processing step, which may be, for example, the evaporation step 101. A solid particle ejection device 151 installed in step 150 captures fiber-containing and mixessludges and other solid materials, and for this purpose,into the fire liquor fed to the recovery boiler 102.
    According to a particularly preferred embodiment, which illustratesin Figure 1 and which gives particularly good results, the second crude pine soap fraction is transferred to a second mixing device.160, where it is mixed with wash water so that a second is dilutedfraction is formed. Then this second diluted fraction is addeda second centrifugal separation step 170, which may be similar to the step150, and which is arranged to perform a separation of the otherdiluted fraction, using a second centrifugal separator.which, like step 150, are preferably imitated byclosed type, so that a third raw soap fractionkoms. This third raw soap fraction contains lower levels ofApplication text 2014-12-10 140030ENblack liquor than the other raw soap fraction, and is thusrelatively clean, preferably cleaner than the other crude pine soap.the fraction.
    Using two series-connected, preferably hermetically sealedcentrifugal separators 150, 170 can be a raw soap with onlyvery small amounts of polluting black liquor are produced, at a relatively low cost and low installation surface requirements.
    In addition, the purification process only takes a short time.
    The preferred overpressure for the second centrifugal separationtower 170, if used, is propagated from apressurized output of step 150, alternatively provided withby means of an additional, in itself conventional, pump betweengoat 150 and step 170.
    A launching device 171 is arranged to catch solidsparticles, such as fiber-containing sludge, and bring this toincreased 102.
    The separated third crude soap fraction is passed on to thethe treatment step 180, in which the raw pine soap is treatedacid as above, to produce tall oil, which thereafteris carried out to a step 105, such as a further treatment step,such as distillation to additional tall oil-based substances,or a use step for the tall oil as a raw material in variousprocesses. Step 105 may be located elsewhere. exceptstep 105, it is preferred that all parts illustrated in Figure 1 be locally arranged parts of one and the same localfacility. In particular, it is preferred that the ash in thethe solution, if used as a washing liquid, consists of ashoriginating from the recovery boiler 102 which forms part of the same system100 to which the reindeer steps 150, 170 belong.
    Application text 2014-12-10 140030EN16The residual acid used is pH-adjusted, in step 181, to becomealkaline, and recycled to the mixing step 160. In case the ash solution from step 104 is used as a wash liquor, the ash solution is pH adjusted accordingly, to be basified.sis, in step 104. It will be appreciated that step 181 thus eitheris connected only to step 180, only to step 104or, if a mixture of residual liquid and ash solution is used or if a selectivity is desired regarding the choice of washable liquid.to both step 180 and step 104. In case of ash releasetype, used only as wash liquor, the residual liquid, from step 180, may instead be fed to the evaporator 101 or some step upstream thereof.
    According to a particularly effective embodiment, illustrated in Figure 1, the wash liquor is carried in a countercurrent circuit in a ratio ofto the raw soap. Thus, in this embodiment, dental fluid supplied to the mixer 140 is comprised of liquid liquid which in a first stage is separated from the second crude soap fraction in step 170. In other words, the output of the heavy fraction of stage 170 is connected to one input of the mixing device 140. In this way, the wash liquor from stage 181 can be used first once in the second separation stage 170, and there occupy a certain proportion of black liquor separated from the second diluted fraction, and then reused in the first separation stage 150, by occupying larger proportions of black liquor from the first dilute the mixture. Since the available amount of residual acid from one and the same plant for crude oil separation and handling, alternatively the availableAlthough the amount of ash from the recovery boiler 102 is limited, this solution offers a very efficient use of the available liquid water wash, which at the same time offers very good results in terms of a final crude soap product with only low proportions of black liquor. In the case of ash removal used as wash waterIn addition, the washed raw soap contains layersApplication text 2014-12-10 140030EN17 amount of precipitated lignin, since the ash solution, unlike the residual acid, does not contain any such precipitated lignin. In general, the invention offers that two different system residues can be used, depending on availability and desire, to provide a high quality end product.
    If the centrifugal separator 170 is not used, the wash water is useddirectly from step 181 to step 140.
    According to the invention, further, the first centrifugal separator is 150,170.and preferably also the second centrifugal separator of the purifier type. This gives a very good purification, especially when two such series-connected centrifugal separators 150,170 of the purifier type are used together on the above-describedsat.
    As described above in connection with the launching device131, 151, 171, it is preferred that at least the first centrifugal separator 131,l5l,and preferably all the centrifugal separators 131, 171 used to provide the respective crude soap fraction (such as the above-mentioned first and second crude soap fractions, which are produced by the separator soap).150, 170), also provides a separation of a respectablea fraction containing solid material comprising fibers and possibly also precipitated salts, which solid-containing fraction is separated and removed for further treatment,as in step 102.
    It is especially preferred that at least steps 140 and 150,but preferably also steps 160, 170, as well as preferablystep 130 and also step 120, are performed continuously. Hari skathe term "continuous" is understood to mean that the various steps 120, 130, 140, 150, 160 and 170, respectively, maintain a continuousstream of inflowing and outflowing fractions, as opposed toApplication text 2014-12-10 140030EN18drives intermittently or batchwise. It is understood that interruptions formaintenance, cleaning and so on can be done, but the main operation is preferably performed continuously. Furthermore,140,there are leveling tanks (not shown in figure 1)between the various continuously operated stages 130, 150, 160, 170. It is preferred that the total throughput time of separated crude soap which arrives at the mixing stage 140, until the washed crude soap arrives at step 180, more preferablyis a maximum of 60 minutes, preferably a maximum of 30 minutes,maximum 10 min.
    In particular, according to this embodiment, a continuoussupplied stream of the first crude soap fraction, which is continuously mixed with the wash liquor in the first mixing device 140, and separated in the first centrifugal separation step 150 to result in the second crude soap fraction. Further, the second crude number soap fraction is mixed in a continuously supplied stream with the wash liquor in the mixer 160 and separated in the second centrifugal separation vessel.step 170 to result in the third raw soap shipmentions.
    As the process is operated continuously rather batchwise, the total capacity can be made to be sufficiently highwith relatively small, continuously operated devices.
    According to a preferred embodiment, only pH-adjusted is usedwash water to wash the raw pine soap during continuousoperation, while, at an initial stage of the procedure, insteadan aqueous solution of sodium sulfate is added to the firstthe mixing device 140 instead of washing water, and possibleto the second mixer 160 instead ofwash water. It will be appreciated that, in the above-describedApplication text 2014-12-10 140030EN19the aqueous liquid circuit, said aqueous solution of sodium sulphate during the initial stage can be supplied only to the second mixing device 160 instead of the washing liquid, and that the separated heavy phase from the second separation-which then contains a black liquor contaminated oneincreased 170,aqueous solution of sodium sulphate, can be fed to the first mixing device 140. It is also possible to use in such an initial stage, instead of said aqueous solution of sodium sulphate, an ash solution as above. This goes to the following. In the case where ash solution is used as wash water, the can solution in question simply continues to be used after the initial stage. In that case pH-adjusted residual acidused as wash water can, after the initial stage, the choiceof washing water of others from ash solution to residual acid.
    According to a preferred embodiment, substantially all of the volume of wash liquor supplied to the mixers 140, 160 either from the tall oil producing process stage 180 or from the recovery boiler 102 and via stages 103 and 104, after pH adjustment in stage 181, and substantially all of the resulting crude soap fraction, most downstream separation stage 170, is passed to the tall oil producing process stage 180 for further processing. With the present system and method it is possible to achieve a very good purification of the crude pine soap and at the same time be limited to only the wash liquor which is formed during the splitting of the purified crude pine soap into pine oil, alternatively which is available fromthe ash from the recovery boiler 102.
    It is preferred that each series-separated separation step 150,170 remove at least 70% by weight, more preferably at least 80% by weight, of the mixture diluted in the respective diluted mixture.held black liquor.
    Application text 2014-12-10 140030ENBoth steps 150 and 170 may comprise a single respective, or several parallel connected centrifugal separators, all of which are preferably of a hermetically sealed type. It is preferred that the total capacity of each centrifugal separator in steps 150, 170,150, 170,rather the total capacity in each stepat a maximum of 70 n§ / h.
    In one example, black liquor from the boiling step 110 was treated ina pulp production process according to the sulphate method, in an initial coarse separation step which in turn included an engravimetric separation tank 120 and a thickening system comprising several series-connected tanks 135, which resulted in a first fraction of 1000 l of raw pine soap, containing 100 l of black liquorated liquid. The free liquor consisted mainly of black liquor, and the black liquor-mixed raw pine soap consisted of "solid" raw pine soap with a certain"Enclosed" content of 35% black liquor.
    Thus, the 1000 l of raw pine soap contained a total of 415 l of black liquor, both in "free" form and in a form "enclosed" to the raw soap. The black liquor contained in the 1000 l of raw soap contained in turn a certain proportion of solid material, in the form of fibroussludge.
    The 1000 l of crude soap was treated with a system 100 as illustrated in Figure 1, in which two series connected centrifugal separators 150, 170 washed the crude soap with the aid of a countercurrent circulating wash liquor in the form of basic residual acid from step 180. After an aqueous solution of sodium sulfate stage is fed to the second mixing device 160, then and then instead of to the second mixing device 160 called washbasin, when the continuous operating process has been allowed to start. In total1500 l of basic residual acid are used.
    Application text 2014-12-10 140030EN21When all the raw soap had been purified, about 94.1% of the totalthe black liquor contained in the raw soap was deposited, together with the corresponding proportion of the solid particles contained in the raw soap contained.
    The end result for a similar experiment is only onecentrifugation step 150 was used, was about 78.3% degradationof black liquor.Vid. a subsequent tall oil producing step 180 was then made from tall oil from the purified tall oil soap, treated with sulfuric acid. Thereafter, the obtained pinethe oil in a further centrifugation separation step, which, among other things, removed fibrous sludge as solid particles, which were removed by ejection from the centrifuge in question. Out-the firing volume was 28 l.
    Corresponding experiments with ash removal from step 104 give similar results.
    The tall oil, if a conventional method had been used in which the crude tall oil had been separated only by auxiliary gravimetric separation, would contain a total of about 560 l of fibrous sludge, which would then need to be removed by such ejection. In the case of the raw soap soap flow of 10,000 l / h of raw all-soap, it had been required that launching be challenged every three minutes during continuous operation. In the example of a centrifugal separation step 150 according to the invention, meanwhile, a total of only 121 l of fibrous sludge was found, which meant that ejection had to be performed only about every thirteenth minute atcontinuous use. In the example according to the invention. with. twoApplication text 2014-12-10 140030EN22 centrifugal separation steps 150, 170, a total of 33 l of fibrous sludge was found, and ejection was necessary only aboutevery fifty minutes.
    Being able to carry out sludge slurry more significantly entails significant benefits in the form of the required service life of the tall oil cleaning centrifuge, as well as the possibility of increasing the capacity of the sludge oil plant since the sludge firing frequency is alimiting factor.
    In addition, less harmful sulfur water is formed during acidification of the waste soap in the splitting plant for tall oil production.the more black liquor that is washed away before this step.
    Above, preferred embodiments have been described. However, cantalamic modifications are made to these embodiments withoutdepart from the fundamental idea of the invention.
    For example, additional initial coarse separations may be performed in the described 120, 130. The outlet from step 150 for the separated heavy fraction (black liquor) may additionally102,instead of being fed to the recovery boiler, it is returned to step 120, for recovery of anyraw soap lost in separation step 150.
    In addition, other types of separators than those illustrated in Figures 2-3 can be used. However, it is preferable not touse some separators of the so-called basket centrifuge type.
    Figure 1 illustrates two series-connected first and second centrifugal separation steps 150 and 170, 130, 135.after the first coarse separation step 120, however, it is also possibleto arrange several series-connected centrifugal separation stepsApplication text 2014-12-10 140030EN23two, such as three, four or more. These are then connected in series, as described above in connection with steps 150,170, preferably with a countercurrently connected wash.
    Residual products from step 180 can be returned to step 120, alternatively to step 101.
    Thus, the invention should not be construed as limited to the embodiments described above, but may be varied within the scope of the invention.the appended claims.
    Application text 2014-12-10 140030EN
    权利要求:
    Claims (15)
    [1]
    A process for purifying crude pine soap from black liquor, using wash liquor, which wash liquor either originates from a tall oil producing process step (180) in which crude pine soap is treated with acid to form tall oil, the wash liquor being constituted by an acidic residual water phase from this process step (180). regulated, or alternatively that the wash liquor consists of a pH-regulated aqueous solution of ash, whereby black liquor-containing crude pine soap is mixed with said wash liquor, and wherein crude pine soap is subsequently separated from the resulting mixture, characterized in that the process comprises the steps of a first coarse separation (120,130) of crude soap from said black liquor to form a first crude soap fraction; b) mixing (140) the first crude soap fraction with wash liquor to form a first diluted fraction; and c) performing a separation (150) of the first spout fraction, using a first purifier-type centrifugal separator, so that a second crude soap fraction is obtained, the second crude soap fraction containing lower levels of black liquor than the first crude soap fraction.
    [2]
    The method of claim 1, wherein the method further comprises the further steps of mixing (160) the second crude soap fraction with wash-liquid to form a second diluted fraction; and e) performing a separation (170) of the second diluted fraction, by means of a second centrifugal separator of purifier type, so that a third raw soap fraction is obtained, the third raw soap fraction containing lower levels of black liquor than the the second raw soap fraction.
    [3]
    3. A method according to claim 2, characterized in that the wash liquor supplied in step b) consists of wash liquor separated from the second crude soap fraction in step e).
    [4]
    A method according to any one of the preceding claims; k ä n n e - t.e c k n a t a v that the wash liquor consists of ash from a recovery boiler (102), which ash is dissolved in water and pH-regulated.
    [5]
    5. A method according to claim 4, characterized in that the wash liquor has a dry matter content of at least 8%, more preferably between 8-22%, more preferably between 13-37%, preferably about 15%.
    [6]
    A method according to any one of the preceding claims; know -that the first (200; 300), (200; 300) drawn and in the applicable centrifugal separator, comprise- (230; 330) (242; 342) cases also the second takes respective separating plates active to separate a relatively heavier phase from a relatively lighter phase (24l; 34l), and that both centrifugal separators operate at at least 1000 rpm.
    [7]
    A method according to any one of the preceding claims; know that the first (300), (300) t e c k n a t a v and i. applicable cases of the second centrifugal separator, are of the hermetically sealed type.
    [8]
    A method according to any one of the preceding claims; can be drawn that at least the first centrifugal separator (200; 300), the rotor and preferably all the centrifugal separators used to produce a respective crude number soap fraction, also provide a separation of a respective Application text 2014-12-10 140030EN 26 fraction. containing solids such as. separated (351) and removed for further treatment. k ä n n e - (120,130)
    [9]
    A method according to any one of the preceding claims, characterized in that the first coarse separation comprises a separation of a raw soap fraction by means of a centrifugal separator comprising separating plates (230; 330) operative to separate a relatively heavier phase (242; 342) from a relatively lighter phase (241; 341), which centrifugal separator operates at at least 1000 rpm. k ä n n e - (120,130)
    [10]
    A method according to any one of the preceding claims, characterized in that the first coarse separation comprises a separation of a crude number soap fraction with auxiliary (120), (130). of gravimetric separation in a tank and a subsequent initial centrifugation step
    [11]
    Method according to one of the preceding claims, characterized in that steps kn and c fl, and in applicable cases also steps d) and e), are carried out continuously, so that a continuously supplied current of the first crude soap fraction from the step a) continuously mixed (140) with the wash liquor in step b) and separated (150) in step c) to re- and in applicable (160) starch in the second crude soap fraction, in case the second crude soap fraction is mixed in a continuous supplied with the wash liquor in step d) and separated (170) in step e) to result in the third crude soap fraction.
    [12]
    Process according to any one of the preceding claims, characterized in that an aqueous solution of sodium sulphate is used in step b), and in applicable cases also in step d), instead of washing water in an initial stage of the process.
    [13]
    Application text 2014-12-10 140030EN 2713. Process according to one of the preceding claims, characterized in that the wash liquor supplied in step b), and in applicable cases also in step d), of 10-14, has a pH value preferably around 11-12.
    [14]
    A method according to any one of the preceding claims, characterized in that substantially the entire volume of wash liquor supplied to grains from said tall oil producing process (180), alternatively comprises lost ash which in its entirety (102), steps grains from a recovery boiler and of substantially all of the resulting crude tall soap fraction, being transported to the tall oil-producing process step (180) for further processing.
    [15]
    A system (100) for purifying crude pine soap from black liquor with which the wash liquor either grains (180) of pine soap is treated with acid to form tall oil, aided by a wash liquor, from a tall oil producing process step in which the crude waste liquid consists of an acidic remaining water phase process step (180) which is pH-regulated, or alternatively that the wash liquor consists of a pH-controlled aqueous solution of ash, (100) wherein the system is arranged to mix black liquor-containing crude pine soap with said wash liquor, and then to separate raw pine soap from the resulting mixture, characterized in that the system (100) comprises) a first coarse separation step (120,130), arranged to separate raw soap from said black liquor so that a first raw soap fraction is formed; b) a first mixing step (140), arranged to mix the first raw soap fraction with wash water so that the first diluted fraction is formed; andc) a first separation step (150) comprising a purifier type first centrifugal separator, which separating step (150) is arranged to separate the diluted fraction of the first application, with the aid of the first centrifugal separator, so that a a second raw soap fraction is obtained, the system (100) being arranged so that the second raw soap fraction contains a lower content of black liquor than the first raw soap fraction. Application text 2014-12-10 140030EN
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    同族专利:
    公开号 | 公开日
    CA2970253A1|2016-06-16|
    WO2016093765A1|2016-06-16|
    RU2017123084A3|2019-06-19|
    SE538684C2|2016-10-18|
    US20170327770A1|2017-11-16|
    RU2017123084A|2019-01-10|
    EP3230422A1|2017-10-18|
    EP3230422A4|2018-07-11|
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    法律状态:
    2020-07-28| NUG| Patent has lapsed|
    优先权:
    申请号 | 申请日 | 专利标题
    SE1451515A|SE538684C2|2014-12-10|2014-12-10|Procedure and plant for washing raw soap|SE1451515A| SE538684C2|2014-12-10|2014-12-10|Procedure and plant for washing raw soap|
    US15/533,132| US20170327770A1|2014-12-10|2015-12-09|Method and system for washing of crude tall oil soap|
    RU2017123084A| RU2017123084A3|2014-12-10|2015-12-09|
    EP15868244.3A| EP3230422A4|2014-12-10|2015-12-09|Method and system for washing of crude tall oil soap|
    PCT/SE2015/051320| WO2016093765A1|2014-12-10|2015-12-09|Method and system for washing of crude tall oil soap|
    CA2970253A| CA2970253A1|2014-12-10|2015-12-09|Method and system for washing of crude tall oil soap|
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