• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Abstract: This invention concerns a continuous method and an arrangement for separation of crude tall oil (CTO) from black r.) liquor. The method involves art initial separation within a tank and/or within a centrifugal separator, and processing of the thus separated taIl oil soap product by aeidulation and/or splitting, followed by ftuther separation, es, by centrifugation. The black p. liquor fraction may be processed for further CTO retrieval, before evaporation and feeding to a recovery boiler.
    公开号:SE1250812A1
    申请号:SE1250812
    申请日:2010-12-28
    公开日:2012-09-28
    发明作者:Anders Goeran Hofstedt
    申请人:Anders Goeran Hofstedt；
    IPC主号:
    专利说明:

    WO 2011/081587PCT/SE2010/0003 TITLE OF THE INVENTION:corrkint10604 sera/424i*** oi A Method of Separating, from a Mixture of Black Liquor and Tall Oil S41ap Product, 10 Concentrated Portions of Tall Oil Soap Product and Arrangements for Said Concentrated Tall Oil Soap Product and/or Separated Black Liquor TECHNICAL FIELD OF THE INVENTION On the one hand this invention generally refers to a method and on the other hand to different arrangements for carrying out the method.
    More specifically the present invention is concentrated to separating, in an introductory or first processing step, from an available mixture of black liquor and small portions of tall oil soap product, concentrated portions of said tall oil soap product from ct 44900.413161•6 serieblack liquor.' Said separated concentrated portions of said tall oil soap product-goad-84par 25 rated-Iga4144iquor.being adapted, within a subsequent or second processing step, for being the object of treatment or processing, such as within an acidulating and splitting y, arrangement to split said concentrated tall ' soap product into crude tail oil .(4-T.9) and *paroled toteAU Liprer teent 44ohyloo into residual products, such as acidic water anclier-the-objeet oftreatment or processing, such as within an evaporation plant and%ucceeding burning in a recovery boiler.
    The crude tall oil within the tall oil soap product is also called CTO, as an ab- breviated expressioniwhich will also be used in the following and in the accompanying drawings.
    CTO is a bi-product from the manufacture of chemical pulp that is obtained from tall oil soap product as a dark odorous liquor before refining, that contains princi- 3 pally resin acid and fatty acid (as oleic acid and linoleic acids) with some sterols and other nonacid components.
    WO 2011/081587PCT/SE2010/0003 2 c5eparetei) 0,0a The present invention is concentrated to purify the concentrated tall oil soap as product and minimize the residual products, such as black liquorQfractions, and to pro- ducetack liquorliwith low tall oil soap content.
    The present invention is thus concentrated towards; on 3o a. A method and an arrangement for separating concentratesi tail oil soap product from black liquor within a first processing step. b. A method and an arrangement for treating or processing thus separated tall oil soap product in a subsequent or second processing steppto form CTO and residual products, such as acidic water and other components and c. A method and an arrangement for treating or processing thus separatediblack liquor, with only a small portion of tall oil soap product, in a subsequent 4:* .seeeo€1 processing step by using an evaporation plant and a subsequent burning of evaporated °black liquor within a recovery boiler.
    Residual products are usually in the form of precipitated lignin and/or salts in a mixture.
    The invention intends thereby to reduce and/or to eliminate the technical problems which are related to the fallout of the tall oil soap product itself and which have turned out otherwise to become of interest in a subsequent acidulating or splitting process for the extraction of CTO from a refined and concentrated tall oil soap product 20 and separate any residual products, where the CTO is directly adapted for a subsequent cleansing or preparation processing step.
    This invention may have advantages for use in a pulp mill based on the sulphate methodiwherein the contents of a digester are permitted to pass over to straining equipment or a straining arrangementiin which fiber-containing products are separated 25 for use in the basic production of pulp, whereas the'131ack liquor formed In the digester is transferred, together with its portions of tall oil soap product4to a separating and concentrating procedural step with regard to said tali oil soap producl here designated as ram) Ro coske an introductory or a first procpdaral or processing step."Wady 1;50ok. tfrOM *SI diqtyko Black liquoP does not only contain sodium and calcium in the form of dissolved salts (for example calcium ions) and lignin compounds but also portions of tall oil soap product, wherein the portions of tall oil soap product has been discontinuously separated to a more concentrated, and from black liquor, more purified form.
    S .
    Such separated, concentrated (thickened) and purified tall oil soap product mil, via an acidulating or splitting process in an acidulating system or arrangement, form WO 2011/081587PCT/SE2010/0003 3 CTO and residual products, such as acidic water, with deposits of salt (CaSO4 and Na2SO4) and lignin compounds or components.
    The present invention makes use of one or more centrifugal separators, for separating in one or more steps portions of tall oil soap product from theV blackliquor, 5 these centrifugal separators are machines that are able to separate mixed substances of different densities by centrifugal forces.
    BACKGROUND OF THE INVENTION Methods, arrangements and structures related to the technical field mentioned 10 above and having a function and a structure which fulfill set requirements are known earlier in a plurality of different embodiments.
    It is previously known that if separated tall oil soap product, within a first processing step, in a mixture of tali oil soap product and black liquor, is exposing a high content of residual products, such as in the form ofiblack liquor a further separation is usually needed before the concentrated tall oil soap product are to be subject to acidu- lating and/or splitting processits.
    It is previously known that if separated black liquor, within a first processing step, in a mixture of tall oil soap product andllack liquor7with a high content of residual products, such as tall oil soap product, causes challenges in an evaporation plant as the evaporated black liquor contains a high portion of tall oil soap product with a too high energy content for a fixed dimensioned recovery boiler.
    With this in mind it has been a challenge to cause a separation of tall oil soap product from black liquor in such a degree that the separation result exceeds the results achieved by X gravimetric separation with one or more tanks and with a discontinuous process.
    As an example of the background of technology and the technical field to which the present invention relates, a method and an arrangement may be mentioned having portions of tall oil soap product separated from the black liquor by means of a discontinuous gravimetric separating process in one or mare tanks, equalizing the flow and uti- 3 0lized in a paper pulp mill.
    Such a separating process is based on that the tall oil soap product, being lighter than the black liquor and its content of tall oil soap product is floating upwards towards and being collectable at the upper portion of a tank, whereas thelplack liquor° sinks downwards and is collectable at the bottom portion of the tank.
    WO 2011/081587PCT/SE2010/0003 4 The previously known technology indicates skimmimg off and separating said it tall oil soap product from available 'black liquor and concentrating the tall oil soap product gravimetrically in a number of procedural steps and thereafter acidulating the tall oil soap product into CTO and acidic water, with its salt and lignin deposits.
    In the publication HUIBERS, D.T.A."Tall Oil" (Kirk-Othmer Encyclopedia of Chemical Technology. John Wiley & Sons, 2000) is a method and an arrangement shown and described which can be considered completely to concur with known arrangements, such as the one illustrated in Figures 1 and 2, respectively in the following and attached drawings.
    In consideration of the characteristics related to the present invention with re- gard to utilizing centrifugal separators, the contents of patent publication US-2,227,203A should be mentioned as the standpoint of earlier technology.
    With regard to the contents of this patent publication a process is shown and described there, for the extraction of tall oil soap produchronn black liquor, in different processing stages or steps, which initially is to have been stored for a gravimetric sepa- ration in a tank (10).
    The process indicates the utilizing of a plural-stage evaporation process in an evaporator plant (11) to a dry substance (DS) of approximately 40 %. swat ThAlack liquor! thickened in this manner with its tall oil soap product and corn- ponents, is supplied to a first centrifugal separator (12), which has the first run-off prod- ucts in the form of black liquorsent to an evaporation stage or plant (24), with DS of 70 %, supplied to a recovery boiler in a known manner.
    More specifically it should be noted that other separated productsjin the form of to tlie tall oil soap product mixed with black liquor, lignin and other residual products, are supplied to a (second) tank (13) for saponification, but through a time-consuming and energy-consuming specific washing and treatment process.
    For this purpose the treatment process indicates that hot (heated) water (15) is supplied to a tank (13) for diluting and dissolving the black liquor and its tall oil soap product over thermal processes, so as thereafter to supply to this diluted and heated solution an alkaline solution (heated solution) for additionally diluting the solution in the tank (13) with the purpose of depositing dissolved saponificated components and/or components that may be saponificated.
    This tall oil soap productjdiluted in two different sequences separated in timejis now to become the subject of an additional centrifugal separation, in a (second) centri- _ • lit • .... ;pc , I., _ a,a first processmg step "ii,1", whichin Figure 34indLcates the use of a gravirnet- ric separation tank ('T") for a continuous separation of a small amount of tall oii , soap products from a large amount ofliack liquor and a centrifugal separator ("C1 n) for further separating the separated tall oil soap products to a lesser amo- unt ofliquor“and• iri Figure 41indicates the use of one or a number of parallel oriented centrifugal separators ("Cla"), to separate a small amount of tall oil soap 40. products from a Large amount of black liquor, b,LA .;Lecond proc-ssIng step "A,3", whichoin Figures 3 and 41indicates a process for continuous treatment of said separated small amount of tall oil soap products ------- to form crude tali all soap products (CTO) and acidic water in a centrifugal separator, _ _ . _ - . -. riti 1,' 0 .i ■ -' - NM, EN .._ .. ._ _ n f a cv- , r r. . . - Dl.GobleA.D.,Self-cleaningcentrifugeimprovesCTO —...,;.., _ separationefficiency,yields,Pulpandpaper,1980,Nov., pp.147-151) WansbroughH1.,Talloilproductionandprocessing, retrievedfromtheInternet,.Copyright2005-2008, www.nzic.org.flz) and W0.2004074415 Al +f-Af g)tAL.4 sea:. *. *tali' o,r.s. ,Aeloani 14_13„, __ olumn 121%a ._ ,v.,rstAIA.c. -- e is , P 01 Cavil: _ I . _L _ ■•■ 58 .re first three lines The use of a cen trifuge for tall oil recovery led to the development of a fully continuous (second processing step ''A3") acidulation process in the mid-1950s" focuses on Plf previously described second processing step ("A3").
    Nothing is mentionedonot even suggestedjin the cited publication "Dl" of any continuous process adapted for and within the first processing step (A1"). it is here described two different processing steps, a first processing step separated from the second processing able step, and which are not directly interconnecte4 with one another.
    It is mentioned, in the publication 'Dl" (Lines 4 to 9), that the oritinuoup system, according to Figure 3 in the cited publication, is using a soap skimming process from a plurality of black liquor tanks and transferring skimmed tali oil soap products to one or several large soap-storage tanks.
    The use of soap skimming processes within sequentially oriented black liquor tanks 4a4- within the first processing step ("Al') clearly points towards the prior use of a dis-continuous separation process. _ • 2e—,21,444:414..w4=4:1° ••• la 1.1...'4.
    It is also mentioned in said publication "Dl" that the tall oil soap products are held in these biack liquor tanks for a long, temperature reducing, period &firms, usually so long that the stored tail cii soap products ends up at low temperatures of 120 to 1°F (50 - 5°C) (in consequence to the long storage time energy losses occur) to allow "black liquorwto separate from the floating tali oil soap products, by a subsequent time-consuming gravimetric separation.
    It is also mentioned that it is important to remove as much black liquor as possible from the separated tall oil soap products before treated in an acidulation arrangement, because the black liquor contains a large amount of dissolved lignin, which will precipitate during the acidulating process.
    To separate and remove as much black iiquid as possible from the separated tall oil soap products in said first processing step "Al" using a number of tanks, each based upon gravimetric separation, as stated above, is not only a very time-consuming but also a temperature -reducing method. This process usually needs an extra energy to raise the temperature before entering the separated tali oil products to said second processing step, products has not been suggested and has considered to be very essenquality of separated tall oil soap products is decreasing notording to a time-related function but also according to a te ure-related function. This is easily compen- sated for by arrelation between the first and the second processing steps €7144Jil 60 WO 2011/081587PCT/SE2010/0003 fugal separator (16).
    The tall oil soap product at that time diluted and separated, is then supplied to a new tank (17) with the same treatment process in two different sequences as in the earlier tank (13), a new centrifugal separation is carried out in another centrifugal separator (20), an additional new tank (21) and a terminating centrifugal separator (23), with the purpose of depositing the dissolved sapontficated and/or saponificatable components so as to separate cleansed tall oil soap product from the cleansing liquid (the solution of Na2SO4).
    In this manner, not only supplying hot water (15) to dilute the tall oil soap prod- uct and other residual products in three different tanks (13, 17, 21) and additionally at each tank supplying an alkaline solution (14) for additional dilution and adaptation of the "pH"-value of the solution and thereafter separating the blackliquor from tall oil soap product in four different centrifugal separators (12, 16, 20, and 23, respectively) requires a relatively high supply of energyowith the present day requirement of effectiveness of energy, and also does not provide the characteristics related to the present invention.
    Furthermore, this arrangement requires measures for handling the substantial quantity of washing liquid that is necessary in the various processing stages or steps. In this regard an evaporation plant should be appropriate. 5/1-5c0 STATEMENT OF THE PRESENT INVENTION TECHNICAL PROBLEM Considering the circumstance that the technical contemplations that a person skilled in the relevant technical art must carry out in order to offer a solution to one or 25 more given technical problems are on the one hand a necessary insight into the measures and/or the sequence of measures which are to be carried out and on the other hand a necessary choice of the one or more means that are necessary, on the basis of this, the following technical problems should be relevant in producing the present object of invention.
    Considering the earlier standpoint of technology, as it is described above and illustrated in the accompanying Figures 1 and 2, based on a method and an arrangement, with a discontinuous withdrawal of tall oil soap portions floating on top of and above a heavierublack liquor from a gravimetrically operating separating tank, as an upper thickened layer, as well as additional separation of the tall oil soap product taken out WO 2011/081587PCUSE2010/0003 6 as a thickened layer in subsequent tanks for measuring a discontinuously procured, more thickened and cleansed tall oil soap product is transferred to an acidulating processifor producing CTO and residual products by adding an acid, it should thus be seen as a technical problem to be able to understand the significance of, the advantag- 5 es related to and/or the technical measures and considerations which will be needed for offering a new process and a method with subsequent processing steps and new ar- rangements adapted to this method, whereby: in614Ce3 a continuous withdrawal of con -' -ted po ions of tall oil soap product from 'black liquorto form a concentrated and su ciently cleansed tall oil soap product$ adaptable for producing CTO and/or, producing a cleansed tall oil soap product with a small or insignificant lowering o.of of temperature without necessarily requiring to supply external heat energy and/or, a short period of time between the relevant withdrawal of concentrated tall oil soap product and the production of CTO and/or,cor4inuooS is utilizing an initialt or firstoeparating step to separate portions of tali oil soap productsand to concentrate portions of tall oil soap producefrom black liquor and a directly (or over a buffer tank) thereto connected acidulating or splitting arrangement and/or €oretinvousis e. improved quality to a separated tall oil soap productsand/or, an increasing throughput velocity of black liquor and tall oil soap product and/or, a small portion of black liquor mixed into the concentrated tail oil soap products so as to thereby create a requirement of a smaller portion of acid (euphoric acid) within the acidulating or splitting arrangement and/or, h. separating off available black liquor drained off over screen equipment with in- cluded portions of tall oil soap productaand concentrating the portions of tall oil soap producfto form CTO in a second processing stage, as well as in a direct", or over a buffer tank, following processing step acidulating such extracted and fully concentrated tall oil soap product into CTO and residual products, while re- ducing otherwise normally appearing energy losses and/or adjusting the tall oil soap producfwithin theH blackliquor separated so it does not jeopardize the function of the evaporation plant and causes a low energy supply to the recovery boiler, with an increased function time and/or I.increasing the production within the paper mill if the capacity of the mill is Ii- WO 2011/081587PCT/SE2010/0003 7 mited due to the actual capacity of the recovery boiler fed by evaporated4black liquor with high tall oil soap produckom discontinuously operated gravimetric tanks.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be 0- required for creating an initial4 or firsts processing step, which with a small reduction of temperature can separate and concentrate portions of tall oil soap producefrom'6lack liquor in order to enable the black liquor with small tall oil soap product to be supplied directly to an evaporation plant.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for creating conditions where, in a method or arrangementsia mixture of black liquor and its small portions of tall oil soap product, during a continuous processing step, may be subject to said separation within a tank and/or within a centri- fugal separator, whereby said separated small portions of tall oil soap product is, in a is concentrated form and with small fractions of black liquor, adaptable to a treatment or processing in a subsequent or second processing step, such as formed as said acidulation and/or splitterarrangement, while said blackliquor, and its adapted small fraction of s tall oil soap product, is subject to be fed to said evaporation plant and thereafter fed to said recovery boiler.in *Xi jirri* Froce$763 01.119 There is a t chnical problem in being able to understand the significance of, the advantages rela d to and/or the technical measures and considerations which will be required for cr ting conditions where separated concentrated tall oil soap product, within said tank may directly be fed to a centrifugal separator, for separating tall oil soap product from residual" black liquor.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will it be required for creating conditions where said separated black liquor within said tank I. and said separated black liquor within said centrifugal separator are to be fed to said evaporation plant.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will Ai0 be required for creating conditions where said black liquor and its small portions of tall WO 2011/081587PCT/SE2010/0003 8 oil soap product is, during a continuous processing step, subject to separation within a second centrifugal separator and/or tank, said separated tall oil soap productsare treated or processed in an acidulating and/or splitting arrangement,to form CTO and acidic water separated in a centrifugal separator.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for permitting, within the initial or first processing step over a centrifugal separator, the separated and concentrated tall oil soap productto exhibit improved characte- ristics and qualities, as separating processes. mowed to the ones that concern earlier known gravimetric puri There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be or required for utilizing as said initiaLfirst, and subsequent (second, third, etc.) processing stee one or more, such as two, centrifugal separators or tanks positioned in series or in parallel.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be or, required for utilizing as said initial,lirst, processing step a first centrifugal separator having a high flow capacity and/or separating capacity and adapting, as said following or 20 subsequent second centrifugal separator, a second utilized centrifugal separator to a considerably lower or low flow capacity and/or separating velocity or capacity.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for creating a procedure based on a fewjsuch as solely twos processing steps 25 and a compact arrangementoadapted for performing the methodland which in its processing steps, via individual centrifugal separators, can successively reduce (and eliminate) the existence of salts (for example calcium sulphate (lime)) and lignin prod- ucts in produced concentrated tall oil soap product in the first processing step and in d used concentrated tall oil soap protuct in the acidulating arrangement.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for reducing (or eliminating) the technical problems which in known technology usually exist in the acidulating process activated in the acidulating or splitting arrangement in consequence of salts (for example calcium sulphate) deposited therein.
    WO 2011/081587PCT/SE2010/0003 9 There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for creating a method and an arrangement with a fewisuch as twodFspecific continuously active and mutually co-ordinated and dimensioned processing steps, one for concentrating portions of tail oil soap productand removing portions of black liquor and one for an acidulating process for acidulating the concentrated tall oil soap product by the use of an added acid In the acidulating or splitting arrangement.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be lo required for having the procedure and arrangement comprise a fewisuch as only two, centrifugal separatorvonnected in series and/or parallel with each other but usually with a buffer tank disposed there between.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be saidv;or firs& required for having residual products, extracted from an initiarprocessing step compris- ing tlicentrifugal separator, to be supplied directly to an evaporating plant.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for improving and increasing the separation and concentration capacities of tali 20 oil soap productand adapted acidulating r o'llthrt: in an existing acidulating or splitting arrangement.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for having the portions of tall oil soap producfto be separated and concen- 2 5 trated, in warm condition, from thetlack liquor and for separating in warm condition concentrated tall oil soap productwith a small amount of a so-called intermediate phase and salt deposition as compared to a tail oil soap productseparated and concentrated gravimetrically in separating tanks.
    There is a technical problem in being able to understand the significance of, the 30 advantages related to and/or the technical measures and considerations which will be required in order to understand that a centrifugal separator, separation and concentration of tall oil soap producffrom41,black liquor, will become more reliable and effective as compared to a gravimetrical separation in one or more separating tanks, which will result in that a larger quantity and quality of tail oil soap productscan be achieved and that WO 2011/081587PCT/SE2010/0003 a larger quantity of separated black liquor can be achieved but also, and not least, that • the evaporation of black liquor, separated from said tall oil soap product does not have 11, to be carried out with too much tall oil soap productin the black liquor, which would result in an altogether too high contribution of energy with problems, such as foam in the 0 If evaporation plant as well as the presence of tall oil soap product in the black liquor, along with pulp fibers, accelerates fouling of the evaporator.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for limiting the addition of the tall oil soap product and/or the concentration of • tall oil soap product to a recovery boiler together with the black liquor without decreas- ing the combustion speed, which would be necessary if the"black liquor"separated from the tall oil soap product is too rich in energy with accompanying portions of tall oil soap productli.
    There is a technical problem in being able to understand the significance of, the 15 advantages related to and/or the technical measures and considerations which will be required for understanding that separator separated portions of tall oil soap products fromialack liquorstoffer higher quality to the concentrated tall oil soap produc than has been possible earlier.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for letting the concentrated tall oil soap producf achieved in this manner be transferred in a warm state, via its first centrifugal separator included in the initial or first processing step directly, or by means of a buffer tank, to the following second po,ses. Ot 0 r e processing step, in which the achieved concentrated tall oil soap &mixed with an acid, in warm condition, for being supplied to a succeeding, second, centrifugal separator for separating treated and concentrated tall oil soap productto CTO and residual products, such as in the form of acidic water.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for letting the tall oil soap product6 thus separated and concentrated and trans- ferred to the acidulating arrangement, be chosen to have a high temperature, such as a temperature of above 9°C or thereabouts.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be WO 2011/081587PCT/SE2010/0003 11 a. required for letting acid in heated condition be chosen to have a high temperature, such as a temperature of higher than 90°C, such as 9°C or thereabouts.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for letting the first centrifugal separator, included in the introductory or first pro- cessing step, be chosen with a high separating capacity for tall oil soap products but with small portions of residual products included, with the consistency or reological condition adapted towards porridge or mousse structure, and black liquorawith high portions of residual products and that the chosen velocity or capacity within the subsequent Sacona) 10 processing step including a second centrifugal separator can be chosen to have a lower speed or capacity of separation for treating &finally concentrated tall oil soap products and reduced residual products.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for permitting the tall oil soap product, formed and concentrated in the first cen- trifugal separator, to be chosen with a high concentration and with very small portions of residual products, such as in the form of black liquor, wherein the concentration of tall oil soap produc is to be greater than 80 procent by volume or thereabouts.
    There is a technical problem in being able to understand the significance of, the 20 advantages related to and/or the technical measures and considerations which will be required for introducing a separating buffer tank between the used processing steps, but however, the formed and concentrated portions of tall oil soap product6 should be transferred directly to an acidulating planyor production of CTO, if possible within a chosen short period of time.
    There is a technical problem in being able to understand the significance of, the advantages related to and/or the technical measures and considerations which will be required for choosing and adapting the duration of time so that the portions of concentration of separated tall oil soap productfrom the black liquor and acidulated into CTO in the acidulating or splitting arrangement exhibit a smaller portion of an intermediate 30 phase and/or salt deposits than the case of/ concentrated tall oil soap products achieved by a gravimetric separation of portions of tall oil soap produc from"black liquor° with the help of separated containers or tanks.
    WO 2011/081587 THE SOLUTION 12 31044 ivt 4%4 charocAtx;36°••1 rtN"437 4 ckaitit 4%00 PCT/SE2010/0003 As its startin point the present invention takes the known technology mentioned by way of introd tion in a method or alternatively in arrangements for separating and concentrating °tons of tall oil soap productfrom black liquor in an introductory or first processirig4ep from an available mixture of black liquor and portions of tall oil soap produce with the concentration of tall oil soap product being adaptable for treatment or processing within a subsequent processing step, such as the addition of an acid becoming the object of acidulating into CTO products and residual products, such as for ex- 10 ample acidic water and for/an evaporation plant and/or a recovery boiler.ia se,,,e04.• In order to solve one or more of the technical problems mentioned olaveelgtpft6.14.4 414 present invention more specifically indicates that the known technology is to be supplemented by the utilization of at least a few processing steps in sequence, according to the characterizing portion of cialmlor alternativelj/the characterizing portion of claim 'FA (3.ccorOing t 100 In addition the characteristics disclosed by the sub claims are indicated as pro- posed embodiments falling within the framework of the basic concept of the present invention.
    ADVANTAGES The advantages which primarily must be considered to be characterizing of the present invention and the specific significant characteristics indicated thereby are that prerequisites have been created hereby for separating, from an available mixture of black liquor and portions of tall oil soap product in a liquidized flow, in an introductory or first processing step a concentrating portion of said tall oil soap product from black liq- uor is to be treatable or processable in a subsequent processing step letting thus sepa- rated and concentrated tall oil soap product, by way of a suggestion to a concentration of more than 80 present by volume, be the subject of acidulating to CTO products and residual products, such as i.e. acidic .water in a nidulating or splitting arrangemeland ..,.0.4jreatrrita t .sesi4 ref 0.444sd kW. tlytoor. in for an evaporation plant and/or a recovery boiler.
    The centrifugal separator of the introductory or first processing step may feed directly and continually with a drained"black liqu4'with its portions of tall oil soap prod- ft uct, and from the drained black liquor the portions of tall oil soap produceare separated and concentrated and being supplied, in a consistency of porridge or mousse structure, to the acidulating or splitting arrangement directly or over a buffer tank and for an eve- WO 2011/081587PCT/SE2010/0003 13 poration plant and/or a recovery boiler.
    The subject matter which is to be considered to be characteristic of a methods according to the present invention is disclosed in the characterizing portion of the follow- s ono 2 ing patent claim 1, whereas arrangements for performing the operation of the method of QM the present inventioni asclosed in the characterizing portion of the following patent • ciainiste.100.44 SHORT DESCRIPTION OF THE DRAWINGS The basic prerequisites occurring in a pulp mill based on the sulphate method and a previously known discontinuous procedure or process with an associated arrangement for separating and concentrating portions of tall oil soap produc eflyel44ess ob- 1 tamed from and included in black liquor, produced in a digester, said portions of said tall oil soap producAncluded in the black liquor and/or for gravimetric separation in tanks of concentrated and cleansed portions of tall oil soap produlinto clean tall oil soap producfsand presently proposed embodiments of a continuous procedure or process and an arrangement adapted thereto, exhibiting the significant characteristics related to the present invention, will now be described more closely in an exemplifying purpose with reference to the enclosed drawings, wherein; Figure 1 schematically shows specific portions or sections of a pulp mill, which is active according to the sulphate method, wherein a flow of liquorlin the form of a black liquor with associated and mixed portions of tall oil soap products2 separated In a sieve arrangement as a used boiling liquid from cellulose fibers, Figure 2 shows schematically a known discontinuous time-consuming method for producing, by means of a gravimetric separation within a number of tanks, more and more concentrated and from black liquor more and more cleansed portions of tall oil soap producewhich here, as a final product, are designated as a concentrated CTO product, Figure 3 illustrates the existence of a tank adapted for gravimetric separation of portions of tall oil soap producfm frolblack liquor" and a centrifugal separator connected after a tank, directly or over a not shown buffer tank, for a continuously acting introductory or first processing step for feeding a continuously acting second processing step WO 2011/081587PCT/SE2010/0003 14 with a centrifugal separator, Figure 4 basically illustrates an embodiment of the present invention wherein a single first centrifugal separator (or a number of parallel oriented separators) is utilized as an introductory first processing stepiwhereas a single separation equipment here 5 shown as a second centrifugal separator (or a number of serial and/or parallel oriented separation equipment such as separators) is utilized as a subsequent or second processing step, in the form of an acidulating or splitting arrangement, andif FigLire shows a table concerning gravimetric separation of black liquor and tall oil soap product designated "GS", and a separation "SS" in accordance with the particulars related to the present invention and specifically an embodiment according to Figures 3 or 4, respectively.
    DESCRIPTION OF A PORTION OF A PULP MILL ACCORDING TO THE SULPHATE 15 METHOD Figure 1 shows utilizing a digester "K', which is supplied with wood chips "Ka" and white liquor "Kb" in a known manner.
    The portions "Kc" of chips, boiled in lye "Kd" and boiling liquid, are after a completed process supplied to a screening equipment or a screening arrangement 11, in which boiled cellulose fibers 11' are run off, and light lye or weak lye, in the form of so- called black liquor 20, passes through the screening equipment 11 together with a smaller amount of portions 10 of tall oil soap producewith the cellulose fibers 11' being transported further in known manner for manufacturing pulp.
    The black liquor 20 and its content of.the portions 10 of tall oil soap produA2e, 444 may, as an initial mixture, be processed in a plurality of processing steps 12 i.e. enabling the extraction of portions 10 of tall oil soap product from black liquor 20, which will be described more specifically as a known procedure and an arrangement for this with reference to Figure 2 and in accordance with the directives of the invention with reference to Figures 3, 4, and 5, respectively.' In the processing step 12 in Figures 1 and 2 the mixture (20, 10) of black liquor 20 and portions of tall oil soap productl 0 are separated by a gravimetric separation in a tank 12a, in which a portion 20a of concentrated black liquor 20' is supplied to an eve- *. g poration plant 13, wherein water evaporates and the portion 20a of black liquor 20' is concentrated from processing step 12 to a/concentration 20"b of black liquor vrOter WO 2011/081587PCT/SE2010/0003 This concentrated black liquor eWia Is supplied to a recovery boiler 14, in which organic wood pieces 14a are burned, whereas inorganic compounds are collected as a lower charge 14b.
    The inorganic matter 14b is mixed with water 15a in a mixer 15 for forming so- called green liquor 15b.
    The green liquor 15b is mixed in a mixer 16 with caustic lime 16a, which results in calcium carbonate 16b ($lime), which is supplied to a lime kiln 17. In mixer 16 the green liquor 15b is converted to white liquor "Kb", for use in the digester "K" via a line or pipe 160. 10 DESCRIPTION OF A KNOWN ARRANGEMENT FOR SEPARATING AND CONCENTRATING TALL OIL SOAP PRODUCT PORTIONS FROM BLACK LIQUOR, AC- CORDING TO FIGURE Z.00, Figure 2 now illustrates an arrangement or processing step 12ain which a mixTur-761 of black liquor 20 and portionsffiEV4 of tall oil soap productor portions 10 are supplied to a separating or equalizing tank "T" (12a) for causing through a gravimetric separation a portion of thickened tall oil soap product 10a to part or separate from the portion 20a It of black liquorwhich in its turn sinks downward and is led via a line or pipe 20a' to the evaporation plant 13 and the recovery boiler 14.
    A first separation step occurs in container or tank "T" and the portion 10a of the tall oil soap producf10 is removed discontinually from the upper part of the tank "T" through a line or pipe "T1'.
    The portion 10a in the tank "T" is thus concentrated and is removed additionally from underlying portions 20a of black liquore three illustrated tanks 21, 22, and which are connected in series and which all are intended for creating a successive thickening of the tall oil soap produc ;10a to 10d1towards the upper portions of the tanks for a floatation of tall oil soap producttotiaas.
    Here Figure 2 illustrates three such thickening tanks 21, 22, 23, in which addi30 tional separation steps are carried out for removing further thickened tall oil soap prod- uctl Od with small portions of residual products such a:black liquo7provided with the ...Y.101, Aim, aaba reference numeral 20b and being supplieeto an evaporation plant 13.
    The tall oil soap product 10d is supplied to acidulating or splitting arrangement in which the concentrated tall oil soap product portions 10d is mixed in a mixer with WO 2011/081587PCT/SE2010/0003 16 an acid 24a, such as sulphuric acid, for acidulating the tall oil soap product 10d into CTO 24c and acidic water 24b, however also containing deposits of salt and lignin products as residual products.
    Residual products, related to black liquora20, are removed by means of drainage pipes 20b' in the tanks 21, 22, and 23, respectively.
    The procedure which is described here is discontinuous with a repetition time of approximately one to two times per week with regard to separating the tall oil soap product piatieee 10a from the black liquor 20a in the container or tank "T".
    DECRIPTION OF THE PRESENTLY PROPOSED EMBODIMENTS By way of introduction it is to be mentioned that in the following description ate/ s presently proposed embodiment which exhibit/ the significant characteristics related to the invention and which 1s clarified by the figures shown in the following drawings we have chosen terms and a specific terminology with the purpose of thereby primarily cla- rifying the inventive concept.
    However, in this connection it should be noted that the terms chosen here are not be considered as being limited solely to the terms utilized and chosen here and that it should be understood that each in this manner chosen term is to be interpreted such that in addition it covers all technical equivalents which operate in the same or substan- 2 0 tially the same manner so as to thereby be able to achieve the same or essentially the same purpose and/or technical result.
    Figure 3 shows a portion of an embodiment having a continuous separation tank "T" adapted for gravimetrical separation and a centrifugal separator "Cl", as a first processing step "Alfor separating and concentrating therein the portions 10a1of a tall oil soap 10 to a concentrated tall oil soap product 10a1 f10131 in Figure *awl for acidu- 424,tlecoad lating In a subsequent processing step 7A3" the concentrated tall oil soap product 10b1 in a acidulating or splitting arrangement 24 into CTO 2fic and leave the residual prod- ucts 24b (see Figure 4).arid a seam c* cm et* 141:44er Gli snete pro44443.
    It is to be noted that the present invention discloses that the concentration of tall 9uitjr oil soap product,V is low and rifted within the black liquor 20 and that the centrifugal separator "Cl" is adapted to concentrate the tall oil soap product 10atto—a tall oil soap product stream 10b1.
    It is to be noted that the present invention discloses that the concentration of black liquor 20 from the digester "K" is high and that th9centrifugal separator "Cl" is are ank 'raga lite WO 2011/081587PCT/SE2010/0003 17 adapted to separate this black liquor alone to a cleansed stream 20b1.
    The present invention is disclosing the following features:producli, 2o,00l Said mixture-of black liquor 20 and its small portions of tall oil soap 10 is, during a continuous processing step, subject to said separation within said tank "Ti' andior within Safe centrifugal separator "Cl", whereby said separated small portions of tali oil soap product 10b1 is, in a concentrated form and with small fractions of 'black liquor, subject to a treatment or processing in a subsequent or second processing step "AT, formed as said acidulation and/or splittOarrangement 24, while said black liquor 20b1, and its small fraction of tall oil soap product (10'), is subject to said evaporation plant 13 and thereafter fed to said recovery boiler 14. 6 Separated concentrated gafiproduct 10a within said tank "T" is directly fed to said centrifugal separator "Cl", for separating tall oil soap product 10b1 from residual black liquor 20b1 and said separated black liquor 20a1 within said tank "T" and said separated black liquor 20b1 within said centrifugal separator "Cl" are fed to said evapora- tion plant 13.
    Said black liquor and its small portions of tall oil soap product is during a continuous processing step subject to separation within a second centrifugal separator and/or tank, said separated tall oil soap product are treated or processed in an acidulating and/or splitting arrangement 24 to form CTO 24c and acidic water 24boseparated in on separation equipment such as a centrifugal separator "C2".
    The fundamental structure of a process, a method and an arrangement forseLiga, ,/oktd parating and concentrating portidfilOal riTigure 3 and 10b1 in Figure 4 of tall oil 20ot soap productfrom black liquor 20b1 in a first processing step "Al" from an available 0I,proavoi mixture of black liquor and portions f.213r44/ of tall oil soap 14 and acidulating the con- centrated tall oil soap product 10b1 in a subsequent second process step "A3" is shown in Figure 4.
    As the mentioned first processing step "Al", a single or parallel oriented centri- c:We fugal separato"Cl a", according to Figure 4, ts utilized having high flow capacity and/or separating speed and/or concentration ability, alternatively a tank "T" adapted for gravi- 3 0metric separation, and a thereafter connected centrifugal separator "Cl; according to Figure 31having a low flow capacity and/or separation speed or capacity and/or concentration capability.
    Figure 4 basically illustrates a method and an arrangement for separating from an available liquor mixture of black liquor 20 and small portions f2f*-14 of tall oil soa (ao,lo)pro uctv WO 2011/081587PCT/SE2010/0003 18 preic6is 10 in an introductory or f' st processing step "Al"Iseparating and concentrating the portions 10b1 of tall oil soa 10 from black liquor 20, with concentrated portions 10b1, of tall oil soap producheing adapted for becoming, in a subsequent process step "A3", the object of acidulating to CTO products 24c and residual products 24b, such as acidic ,kprockixt: water.
    The small tall oil0 portions received in this manner is transferred over a first centrifugal separator "Cl a", included in the introductory processing step "Al", in heated condition directly to, or via a not illustrated buffer tank "B", the subsequent process step "A3", wherein the produced concentrated tall oil soap product 10b1 is mixed with an acid 24a, in(a heated stage, for being supplied to separation equipment a a second centrifugal separator "C2" for separating CTO products 24c from resi- dual products 24b, such as in the form of acidic water, precipitated lignin and salts.
    The concentrated tall oil soap product 10b1 transferred in this manner is chosen to have a temperature higher than or at least around approximately 9°C, whereas the 15 acid 24a in warm condition is chosen to a temperature of above or at least around ap- proximately 9°C. Lower values could be accepted than the mentioned values, but higher values are preferred. Figures 3 and 4 have been completed with values representing volumes per hour, concentration values etc as suggested values.
    Figure 4 illustrates that the first centrifugal separator "Cal" included in the intro-20 ductory processing step "Al" is chosen with a high separation capacity for forming a concentrated tall oil soap product 10b1 with small portions of residual products (20') mixed there into, having a porridge or mousse consistency, and separated black liquor 20b1 having an adapted small residual portion of tall oil soap (10') and with separation equipmentIsuch as a second centrifugal separator "C2", included in the subsequent 25 processing step "A3", is chosen with a lower separation capacity for forming CTO products 24c and residual products 24b. In both separation positions the separator "Cie" can consist of several parallel installed separators if the separation capacity requires a capacity larger than one separator can handle.
    The invention proposes that the concentrated tall oil soap product I Obi Is 30 formed in the first centrifugal separator "Cl", "Cl a" and should have a concentration of greater than 80 percent by volume.
    Furthermore, in accordance with the invention, it is indicated that the produced concentrated tall oil soap product 10b1 thus formed is to be transferred to separation equipmentIsuch as a second centrifugal separator "C2"bwithin a chosen short period of WO 2011/081587PCT/SE2010/0003 19 time, preferably shorter than 10 hours, for decreasing or reducing energy losses and for retaining the quality of the tall oil soap producNontained therein.
    More particularly it is indicated that the period of time be chosen and adapted such, that the tall oil soap product 10b1 separated from the black liquor and concen- trated will after treatment in the acidulating arrangement 24 as In separation equipments such as a centrifugal separator "C2 "exhibit a smaller portion of an intermediate phase and/or salt deposits than what applies to a tall oil soap product produced by separating said tall oil soap product from black liquor in a gravimetric tank "T", in accordance with Figures 1 and 2, respectively.
    Figure 5 illustrates In a table the values "GS" pertaining to an arrangement accor- ding to Figures 1 and 2, respectively, and the values "SS" pertaining to a tall oil soap product10b1 produced according to Figure 3 or Figure 4, respectively.
    It is to be noted that the centrifugal separators "Cl" and "Cl a' may have a design where not only concentrated tall oil soap product 10b1 but alsoablack liquor 20b1 is 15 separated.
    Further more the centrifugal separators "Cl" and "Cie" has an additional exit 20b2 intended to separate suspended material having a density exceeding the density of black liquor. This suspended material is directly fed to the recovery boiler 14.
    The invention is of course not restricted to the embodiment disclosed above as 20 an example and it can be subjected to modifications within the frame of the inventive concept illustrated in the following claims.
    It should be particularly noted that each illustrated unit and/or circuit can be combined with each of the other illustrated units and/or circuits within the framework of being able to achieve the desired technical function.
    PCT /5E2010 /0003 -92- 2012
    权利要求:
    Claims (8)
    [1] 1. A method of separating, in a first processing step ("Al"), from an available mixture of black liquor (20) and small portions (10) of te oil soap products, concentrated 0.
    类似技术:
    公开号 | 公开日 | 专利标题
    SE1250812A1|2012-09-28|Procedure for separating portions of tall oil soap product and a plant for this.
    AU2003203072B2|2009-04-23|Distalliative process of extracting and purifying phytosterols and phytostanols from tall oil pitch
    WO2009017389A2|2009-02-05|Method for extracting crude palm oil
    US9085547B2|2015-07-21|Process for autocatalytic esterification of fatty acids
    WO2010101454A2|2010-09-10|Process for extracting palm oil using evaporation
    SE453840B|1988-03-07|METHOD OF PRODUCING CELLULOSAMASSA
    AU5188800A|2001-02-15|Process for treating biomass fibrous material
    EP1442107B1|2006-10-25|Brine separation in tall soap oil preparation
    RU2671534C2|2018-11-01|Method and arrangement for the separation of tall oil products from black liquor
    FI64670B|1983-08-31|AOTERVINNINGSFOERFARANDE VID SULFATCELLULOSAKOKNING
    WO2007146971A1|2007-12-21|Method of refining oil recovered from ethanol processing byproducts
    AU739166B2|2001-10-04|Process for obtaining oryzanol
    SE0901623A1|2011-07-01|Procedure for letting a raw soap from black liquor
    WO2015037980A1|2015-03-19|Zero liquid discharge palm oil clarification process
    EP3305877B1|2022-01-05|Process for purifying biodiesel
    US2417329A|1947-03-11|Method of refining crude wool grease
    EP3825389A1|2021-05-26|A method for producing crude palm oil from a palm-oil containing raw material and a system for the production of crude palm oil
    US2124779A|1938-07-26|Manufacture of starch
    Todd et al.1965|Continuous soapstock acidulation
    CN107964370A|2018-04-27|A kind of technology for producing colophony
    RU2048511C1|1995-11-20|Method of producing fatty acids from soap stock of vegetable oils
    同族专利:
    公开号 | 公开日
    EP2519620B1|2020-04-29|
    US20120296066A1|2012-11-22|
    CA2785779C|2018-01-23|
    CA2785779A1|2011-07-07|
    WO2011081587A1|2011-07-07|
    SE0901624A1|2011-07-01|
    SE537426C2|2015-04-28|
    EP2519620A1|2012-11-07|
    SE534404C2|2011-08-09|
    RU2570710C2|2015-12-10|
    RU2012131912A|2014-02-10|
    EP2519620A4|2014-11-05|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2285902A|1938-06-08|1942-06-09|American Cyanamid Co|Treatment of black liquor soap and the like|
    US2200468A|1938-08-08|1940-05-14|Francis J Cirves|Recovery of by-products from black liquor|
    US2227203A|1938-11-05|1940-12-31|Sharples Corp|Manufacture of soap|
    US2475361A|1946-03-06|1949-07-05|Benjamin Clayton|Process of treating waste pulp liquors|
    SU76379A1|1948-08-02|1948-11-30|В.Д. Худовеков|The method of obtaining in the continuous process of crude tall oil|
    US2838481A|1956-06-29|1958-06-10|Laval Separator Co De|Method for continuous processing of tall oil and the like|
    US3449313A|1965-11-18|1969-06-10|Pulp Chem Ass|Recovery of tall oil soaps from sulfate process black liquor|
    US3890295A|1973-06-15|1975-06-17|Betz Laboratories|Methods and compositions to enhance tall oil soap separation|
    SE386693B|1974-01-11|1976-08-16|Skogsegarnas Ind Ab|MEASURES TO PREVENT OR REDUCE EMISSIONS OF ODOR-SMELLING AND / OR ACID SULFUR COMBUSTION PRODUCTS FROM CHEMICAL REGENERATION PROCESSES IN MASS PRODUCTION BY MEDIUM-ALKALINE EXPOSURE ...|
    US4101535A|1976-04-01|1978-07-18|Hudson Pulp & Paper Corp.|Method and apparatus for recovering saponified tall oil|
    US4238304A|1979-08-30|1980-12-09|Raybestos-Manhattan, Inc.|Method for improved recovery of tall oil from black liquors|
    FI66296C|1983-01-11|1984-10-10|Linotek Oy|CONTAINER SEPARATIONSANORDNING OCH FOERFARANDE FOER SEPARERING AV I EN VAETSKEBLANDNING INGAOENDE LAETTA OCH TUNGA VAETSKEFORMIGA FRAKTIONER|
    US5286845A|1992-05-20|1994-02-15|Union Camp Corporation|Acidification of tall oil soap using carbon dioxide|
    US5635024A|1993-08-20|1997-06-03|Bountiful Applied Research Corporation|Process for separating lignins and dissolved organic compounds from kraft spent liquor|
    US5468396A|1994-03-16|1995-11-21|Pulp And Paper Research Institute Of Canada|Centrifugal cleaning of pulp and paper process liquids|
    FI104491B|1996-12-30|2000-02-15|Aga Ab|Method and apparatus for purifying a crude tall oil filter|
    US6462210B1|1999-04-16|2002-10-08|Harting, S.A.|Fractionation process for the unsaponifiable material derived from black-liquor soaps|
    US6582601B1|2000-01-18|2003-06-24|Andritz Oy|Method and apparatus for separating soap|
    SE0300434D0|2003-02-18|2003-02-18|Kiram Ab|Crude tall oil recovery in alkaline pulp mills|
    US7504478B2|2007-01-26|2009-03-17|Nalco Company|Additives for increasing the separation yield of tall oil soap from black liquors|
    EP2151165A1|2008-08-06|2010-02-10|Nestec S.A.|Multi-Layered Chilled Dessert|SE536962C2|2013-03-20|2014-11-18|Anders Hofstedt|Analysis method for measuring the content of soap in black liquor and an analysis container|
    SE537699C2|2013-03-20|2015-09-29|Anders Göran Hofstedt|Method and plant for separating tall oil products from black liquor|
    SE539191C2|2014-08-21|2017-05-09|Hofstedt Anders|Method and apparatus for separating two phases|
    SE538684C2|2014-12-10|2016-10-18|Göran Hofstedt Anders|Procedure and plant for washing raw soap|
    US11034914B2|2018-05-01|2021-06-15|Kraton Polymers Llc|Desulfurized black liquor soap compositions and processes for producing|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    SE0901624A|SE534404C2|2009-12-30|2009-12-30|Procedure for separating and splitting raw soap from a mixture of black liquor and raw soap|
    SE1250812A|SE537426C2|2009-12-30|2010-12-28|A procedure for separating portions of the tall oil soap product and a plant for this.|
    PCT/SE2010/000320|WO2011081587A1|2009-12-30|2010-12-28|A method of separating, from a mixture of black liquor and tall oil soap product, concentrated portions of tall oil soap product and arrangements for said concentrated tall oil soap product and/or separated black liquor|SE1250812A| SE537426C2|2009-12-30|2010-12-28|A procedure for separating portions of the tall oil soap product and a plant for this.|
    [返回顶部]