• 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:
    A system (10) for treating spent pulping liquor (14) comprising lignin to provide green liquor (47) is disclosed. The system (10) comprises an evaporator (22), a recovery boiler (34), at least one filter (58, 74), and a green liquor plant (46). The evaporator (22) concentrates a first stream (18) of the spent pulping liquor (14) to provide a concentrated pulping liquor (30). The recovery boiler (34) incinerates the concentrated pulping liquor (30) to provide a smelt (42). The at least one filter (58, 74) filters a second stream (54) of the spent pulping liquor (14) to remove lignin therefrom to provide a permeate (66, 82). The green liquor plant (46) is for dissolving the smelt (42) from the recovery boiler (34) in the permeate (66, 82) from the at least one filter (58, 74) to provide green liquor (47). Also disclosed is a method for treating spent pulping liquor (14) to provide green liquor (47).
    公开号:SE1651205A1
    申请号:SE1651205
    申请日:2016-09-08
    公开日:2018-03-09
    发明作者:Arkell Anders
    申请人:Suncarbon Ab；
    IPC主号:
    专利说明:

    Sep 5, 2016; S&G Ref: P139640001 METHOD AND SYSTEM FOR TREATING SPENT PULPING LIQUOR Field of the inventionThe present invention relates to a method and system for treating spent pulpingliquor comprising lignin from a kraft pulping process to recover spent cooking Chemicals.
    Background The kraft pulping process for conversion of wood into wood pulp is wellknown. A white liquor that contains active cooking chemicals including NaOH (sodiumhydroxide) and NagS (sodium sulfide) is used to solubilize lignin and liberate fibersfrom wood chips to produce pulp and spent pulping liquor. The pulp recovered aftercooking the wood is also known as brown stock pulp. The spent pulping liquor is alsoknown as black liquor and contains organic substances, active cooking chemicalsincluding mainly NaHS, NagS, and NaOH as well as spent cooking chemicals includingNagCOg (sodium carbonate), Na2SO4, NaSgOg, and NaSOg. The black liquor isconcentrated in an evaporation plant and is then incinerated in a recovery boiler toproduce steam and a smelt of molten salts that consists mainly of NagCOg and NagS.The smelt is dissolved in water (or a process water known as weak white liquor) toproduce a solution of NagCOg and NagS known as green liquor. The NagCOg in thegreen liquor is then converted to NaOH by mixing the green liquor with calcium oxideto regenerate the white liquor containing NaOH and NagS for use as active cookingchemicals in the pulping process.
    High content of inorganic solids and lignin in the concentrated black liquorfrom the evaporator lead to increased viscosity and may lead to precipitation of solidswhich causes undesired plugging in evaporators and pipes. The evaporation plantcapacity is a function of evaporation of water from the black liquor and the compositionof black liquor. It may desirable to off-load the evaporation plant for example byreducing the charge of spent liquor solutions or aqueous solutions charged to theevaporators in a kraft pulp mill. Higher load of organic material in the black liquor maycause overloading of the recovery boiler. The recovery boiler thus may become a“bottle-neck”, for example, if the mill is planning to increase pulp production capacity.Further, recovery boilers and evaporation plants are expensive to upgrade or to replace.
    Attempts have been made to reduce the load on the evaporator or recoveryboiler to alleviate the plugging and fouling i.e. “off-load” the overall cooking chemicalrecovery process. These attempts have focused on reducing the therrnal load on the recovery boiler since this is usually the bottle-neck of the pulp mill and is the most Sep 5, 2016; S&G Ref: Pl3964000l expensive unit to upgrade or replace. The quantity of organic substances, especiallylignin, in the concentrated black liquor deterrnines the limit at which the recovery boileroperates.
    WO 2013/ 137790 and WO 2016/007550 disclose methods for separating ligninfrom black liquor by acidification then separation of a lignin solid. However, acidifyingthe black liquor increases costs for the requisite acid and alkali since the sodium-sulphurconcentrations have to be balanced and leads to problems with increased purge ofsodium sulphate, such as ash from an electrostatic precipitator.
    WO 2015/ 137861 discloses a method for membrane filtering of black liquor toobtain a lignin fraction having a desired molecular weight distribution.WO 2015/ 121477 discloses a process for treating black liquor involving filtering theblack liquor with a membrane filter, lowering the pH to precipitate organic matter,adding ammonia and an alcohol to the organic matter, and subjecting the solution tocracking. The obtained lignin may be made into a liquid fuel.
    A process for lignin valorization into bio oils by ultrafiltration of spent cookingliquor into various lignin size fractions, acidifying/precipitating the lignin followed bycatalytic depolymerization of lignin fractions is described in A. Toledano et. al.Chemical Engineering Joumal, vol. 193-194, 2012, p. 396-403.
    While systems for recovery and upgrade of lignin in pulp mills are known inthe art, it would be desirable to provide improved systems and methods for reducing theload on evaporators and recovery boilers in pulp mills and allow for valorizing thelignin into useful products whilst continuing to recover substantially all of the cooking chemicals used in the pulping process.
    Summary of the invention Consequently, the present invention seeks to mitigate, alleviate, eliminate orcircumvent one or more of the above-identified deficiencies in the art and disadvantagessingly or in any combination by providing in a first aspect a system for treating spentpulping liquor comprising lignin to provide green liquor, the system comprising: an evaporator for concentrating a first stream of the spent pulping liquor toprovide a concentrated pulping liquor; a recovery boiler for incinerating the concentrated pulping liquor to provide asmelt; at least one filter for filtering a second stream of the spent pulping liquor toremove lignin therefrom to provide a perrneate; and a green liquor plant for dissolving the smelt from the recovery boiler in at least a part of the perrneate from the at least one filter to provide green liquor.
    Sep 5, 2016; S&G Ref: Pl3964000l According to an embodiment, the system comprises at least two filters. A firstfilter for filtering the second stream of the spent pulping liquor to provide a firstretentate and a first perrneate and a second filter for filtering the first perrneate toprovide a second retentate and a second perrneate. According to such an embodiment atleast part of the second perrneate is used to dissolve the smelt in the green liquor plant.The first filter may be a membrane filter with a molecular weight cut-off between 0.5and 20 kDa. The second filter may be a membrane filter with a molecular weight cut-offlower than the one of the first filter. The molecular weight cut-off of the second filtermay be between 0.2 and 0.8 kDa.
    In some embodiments the system comprises at least one filter for filtering asecond stream of the spent pulping liquor to provide a retentate and a perrneate. In theseembodiments the system further comprises a de-polymerization reactor for treating the retentate to provide a de-polymerized lignin stream.
    According to a second aspect there is provided a method for treating spentpulping liquor comprising lignin to provide green liquor, the method comprising: (a) dividing the spent pulping liquor into a first stream and a second stream; (b) evaporating the first stream to provide a concentrated pulping liquor; (c) incinerating the concentrated pulping liquor to provide a smelt; (d) filtering the second stream to remove lignin, thereby obtaining a perrneate with reduced content of lignin; (e) dissolving the smelt in at least a portion of the perrneate to provide green liquor.
    According to an embodiment, the filtering step (d) may comprise at least twofiltering steps. In the first filtering step, the second stream of the spent pulping liquor isfiltered to remove a first portion of lignin to provide a first retentate and a firstperrneate. In the second filtering step, the first perrneate is filtered to remove a secondportion of lignin to provide a second retentate and a second perrneate. Subsequently, atleast part of the second perrneate is used to dissolve the smelt in the green liquor plantin step (e). The molecular weight cut-off is typically higher in the first filtering step thanin the second filtering step. The molecular weight cut-off may be between 0.5 and 20kDa in the first filtering step and between 0.2 and 0.8 kDa in the second filtering step.The first retentate and the second retentate may be combined into a single stream comprising the removed lignin.
    Sep 5, 2016; S&G Ref: P139640001 According to an embodiment, the second stream is between about 5 to 50% byvolume of the spent pulping liquor, preferably about 10 to 50% by volume of the spentpulping liquor. Preferably, the first stream is the major stream and the second stream isthe minor stream. The volume ratio may thus be at least 2: 1.
    In some embodiments step (d) of the method comprises filtering the secondstream to obtain a retentate and a perrneate. In these embodiments the method furthercomprises a step of de-polymerizing the retentate to provide a de-polymerized ligninstream. In embodiments wherein the method comprises more than one filtering step,some but not all of the resulting retentates may be subject to de-polymerization beforebeing combined. By de-polymerization of lignin with higher molecular weight, themolecular weight distribution in the combined retentate will be more narrow. In amethod comprising two filtering steps, the first but not the second retentate may be subject to de-polymerization.
    Brief description of the drawings These and other aspects, features and advantages of which the invention iscapable of will be apparent and elucidated from the following description of anembodiment of the present invention, reference being made to the accompanyingdrawings, in which: Figure 1 is a system for treating spent pulping liquor comprising lignin according to an embodiment.
    Detailed description of an embodiment The following description focuses on an embodiment of the present inventionapplicable to a system and method for treating spent pulping liquor to provide greenliquor. However, it will be appreciated that the invention is not limited to thisapplication but may be applied to other systems and methods which involve treatingspent liquor e.g. soda liquor from a soda cooking process.
    The table below lists features of the system 10 in figure 1.
    Feature Reference numera]System 1 0Spent pulping liquor 14First stream of pulping liquor 18Evaporator 22Condensate 26 Concentrated pulping liquor 3 0 Sep 5, 2016; S&G Ref: Pl3964000l Feature Reference numeralRecovery boiler 34Flue gases 38Smelt 42Green liquor plant 46Green liquor 47White liquor plant 48White liquor 50Second stream of pulping liquor 54First filter 5 8First retentate 62First perrneate 66De-polymerization reactor 70De-polymerized lignin stream 71Second filter 74Second retentate 78Second perrneate 82Combined lignin stream 86Brown stock wash 90 As used herein the terms “spent pulping liquor” and “black liquor” are usedinterchangeably.
    Figure 1 illustrates a system 10 for treating spent pulping liquor 14 from a kraftpulp mill comprising lignin. A method for treating spent pulping liquor 14 will also beevident to the skilled person from the description of system 10.
    Spent pulping liquor 14 is separated into a first stream 18 and a second stream54. As already mentioned, spent pulping liquor 14, apart from lignin, comprises spentinorganic cooking chemicals, such as NagCOg, Na2SO4, NaSgOg, and NaSOg.
    The first stream 18 enters evaporator 22 wherein it is concentrated to formcondensate 26 and concentrated pulping liquor 30. The concentrated liquor 30 thenenters recovery boiler 34 for incineration. Flue gases 38 evolve from recovery boiler 34and a smelt 42 is produced. Smelt 42 is then dissolved in an aqueous second perrneate82 obtained from treatment of the second stream 54 as will be described below. Asalready mentioned, the smelt comprises molten salts that consist mainly of NazCOg andNagS. Additional aqueous liquids or process water available in the kraft mill (notshown) may be used to dissolve the smelt 42 if the quantity of second perrneate 82 is insufficient. Dissolution of smelt 42 occurs in green liquor plant 46 to form green liquor Sep 5, 2016; S&G Ref: P139640001 47 which is re-causticized using calcium hydroxide in White liquor plant 48. Theregenerated white liquor 50, comprising NaOH and NagS, from the white liquor plant 48is recycled back to the wood Cooking plant of the kraft pulping process (not shown).
    The second stream 54 of spent pulping liquor enters first filter 58 whereinstream 54 is separated into a first retentate 62 and a first perrneate 66. The first retentate62 is rich in organic substances, including lignin, while the first perrneate 66 is depletedof organic substances. The first retentate 62 is sent to de-polymerization reactor 70wherein it is treated to produce a de-polymerized lignin stream 71. The first perrneate66 enters second filter 74 to yield a second retentate 78 and a second perrneate 82further depleted of organic substances. Optionally, some of the first perrneate 66 is sentto evaporator 22. Altematively, some of the first perrneate 66 may be used in the woodchip impregnation liquor or reintroduced elsewhere in the pulping process (not shown).The second retentate 78 has a high concentration of substances with a molecular weightdistribution deterrnined by the porosity cut-off of the first filter 58 (upper limit) and thesecond filter 74 (lower limit). Second retentate 78 is combined with de-polymerizedlignin stream 71 to produce a combined lignin stream 86 suitable for manufacture oflignin bio-oil or other useful products. By de-polymerizing the first retentate 62, themolecular weight distribution of the combined lignin stream 86 becomes more narrow.Moreover, the combined lignin stream 86 is homogenous. A homogenous lignin streamwith a lower and narrower molecular weight distribution is useful as a precursor for theproduction of liquid fuels. The second perrneate 82 has a lower concentration of organicsubstances than the first perrneate 66. At least a portion of the aqueous secondperrneate 82 is sent to the green liquor plant 46 for dissolving the smelt 42 as describedabove. Optionally, some of the second perrneate 82 is used to replace evaporationcondensate in brown stock wash 90. It may further be discharged to other positions inthe kraft mill including wood impregnation steps, oxygen delignification steps or to ableach plant unit.
    The first filter 58 and the second filter 74 are membrane filters operating incross-flow mode. The membrane of the first filter 58 is an ultrafiltration membrane oran open nanofiltration membrane with a molecular weight cut-off in the range of 0.5 to20 kDa, preferably about 1 kDa. The molecular weight cut-off of the membrane in thesecond filter 74 is lower than of the first filter 58 and is preferably between 0.1 and 0.8kDa, such as about 0.2 kDa.
    The second stream 54 that is fed to the first filter 58 is typically a weak spentpulping liquor (i.e. black liquor containing about 15% solids) from the wood digestersof the kraft pulping process as described above. Altematively, the second stream 54 may be an interrnediate black liquor (containing about 20-30% solids) from the black Sep 5, 2016; S&G Ref: P139640001 liquor evaporator 22 or a combination of a weak black liquor and an interrnediate blackliquor. An advantage of using an interrnediate black liquor as the second stream 54 isthat rosin soaps have usually been removed from the liquor. The rosin soaps maynegatively affect the filtering process. Further are the rosin soaps a valuable by-product.
    The second stream 54 is between about 10 to 50% by volume of the spentpulping liquor 14. Commonly, the first stream 18 is the major stream and the secondstream 54 is the minor stream. The second stream 54 may be about 25% by volume andthe first stream 18 may be about 75% by volume of the spent pulping liquor 14.
    The present applicant has surprisingly found that the method and system of theinvention significantly reduces the load on both the evaporation plant and the recoveryboiler in a pulp mill whilst simultaneously recovering substantially all of the cookingchemicals for re-use in the pulping process. Avoiding a trade-off between reducing theload of the evaporation plant and the recovery boiler on the one hand, and the recoveryof the cooking chemicals on the other is a major advantage. Thus, the present processallows for pulp production capacity of a kraft pulping mill to be increased whilstdispensing with the need to upgrade or replace the recovery boiler and/or evaporationplant. Further, the method and system of the invention allows for valorizing part of the lignin in the wood into useful products, contributing to the overall process economy.
    Example The system 10 was operated as follows. Weak black liquor 14 from thedigestion of softwood was used. The membrane of the first filter 58 had a molecularweight cut-off of 1 kDa while the membrane of the second filter 74 had a molecularweight cut-off of 0.2 kDa. The weak black liquor 14 was divided into a first stream 18that was sent to the evaporator 22, recovery boiler 34 etc. as described above and asecond stream 54 that was filtered through the first filter 58 operated with cross-flowvelocities between 3 and 5 m/s, transmembrane pressures of 5 to 35 bar and at atemperature between 70 °C and 120 °C. The first filter 58 separated between 75 and 90wt.% of the lignin from the second stream 54. The first retentate 62 had a ligninconcentration between 190 and 280 g/l (compared with 55 to 70 g/l in the initial weakblack liquor 14 and second stream 54). The first retentate 62 was subjected to basecatalysis in de-polymerization reactor 70 at a temperature between 250 and 290 °C forbetween 10 minutes and 4 hours to de-polymerize the lignin. The de-polymerizationreactor 70 may contain one or more catalysts. The catalysts may be homogenous orheterogeneous. The catalyst may be selected from the group consisting of nickel,copper, molybdenum, and zirconium catalysts on a support, calcium compounds, sodium hydroxide, and potassium carbonate. Hydrogen gas, a hydrogen donor solvent, Sep 5, 2016; S&G Ref: Pl3964000l or a solvent such as phenol, cresol, or methanol may also be added to the de-polymerization reactor 70. The molecular weight distribution of the lignin was reducedfrom between 1 and 10 kg/mole in first retentate 62 to between 0.2 and 1.4 kg/mole inde-polymerized lignin stream 71. The first perrneate 66 was filtered through secondfilter 74 at similar conditions to the first filter 58. The obtained second perrneate 82contained lignin and hemicellulose in concentrations of only about 2 wt.% of theirconcentrations in the second stream of black liquor 54. The second perrneate 82 has loworganic content and a high content of cooking chemicals including NagCOg. Further, theorganic compounds in this stream have a low molecular weight (less than 0.2 kDa).Aqueous streams with low content of organic material may be charged to green liquorplants which are not able to tolerate particulate organics in any quantities, though beingequipped with efficient green liquor filters, but rather to tolerate salts and water. Thesecond perrneate 82 was sent to the green liquor plant 46. The obtained second retentate78 contained lignin with a molecular weight distribution between that of the membranefilters i.e. between 0.2 and 1 kDa. This distribution was similar to the lignin in the de-polymerized lignin stream 71. The second retentate 78 was combined with the de-polymerized lignin stream 71 to produce a combined lignin stream 86 suitable formanufacture of lignin bio-oil or other useful products.
    Although the present invention has been described above with reference tospecific illustrative embodiments, it is not intended to be limited to the specific form setforth herein. Any combination of the above mentioned embodiments should beappreciated as being within the scope of the invention. Rather, the invention is limitedonly by the accompanying claims and other embodiments than the specific above areequally possible within the scope of these appended claims.
    In the claims, the term “comprises/comprising” does not exclude the presenceof other species or steps. Additionally, although individual features may be included indifferent claims, these may possibly advantageously be combined, and the inclusion indifferent claims does not imply that a combination of features is not feasible and/oradvantageous. In addition, singular references do not exclude a plurality. The terms “a”, “an”, “first”, “second” etc. do not preclude a plurality.
    权利要求:
    Claims (10)
    [1] 1. A system (10) for treating spent pulping liquor (14) comprising lignin toprovide green liquor (47), the system (10) comprising: an evaporator (22) for concentrating a first stream (18) of the spent pulping liquor(14) to provide a concentrated pulping liquor (3 0); a recovery boiler (34) for incinerating the concentrated pulping liquor (30) toprovide a smelt (42); at least one filter (58, 74) for filtering a second stream (54) of the spent pulpingliquor (14) to remove lignin therefrom to provide a perrneate (66, 82); and a green liquor plant (46) for dissolving the smelt (42) from the recovery boiler(34) in at least a part of the perrneate (66, 82) from the at least one filter (58, 74) toprovide green liquor (47).
    [2] 2. The system of claim 1, wherein the at least one filter (58, 74) comprises: a first filter (58) for filtering the second stream (54) of the spent pulping liquor(14) to provide a first retentate (62) and a first perrneate (66); and a second filter (74) for filtering the first perrneate (66) to provide a secondretentate (78) and a second perrneate (82); wherein the second perrneate (82) is used to dissolve the smelt (42) in the greenliquor plant (46).
    [3] 3. The system of claim 2, wherein the first filter (5 8) is a membrane filter with amolecular weight cut-off between 0.5 and 20 kDa and the second filter (74) is amembrane filter with a molecular weight cut-off lower than first filter (58); preferablythe molecular weight cut-off of the second filter (74) is between 0.1 and 0.8 kDa.
    [4] 4. The system of claim 2 or claim 3, wherein the first filter (58) is a membranefilter with a molecular weight cut-off of about 1 kDa.
    [5] 5. The system of any one of claims 1 to 4, wherein the second stream (54) is between about 10 to 50% by volume of the spent pulping liquor (14).
    [6] 6. The system of any one of claims 1 to 5, wherein the second stream (54) is about25% by volume and the first stream (18) is about 75% by volume of the spent pulpingliquor (14). Sep 5, 2016; S&G Ref: P139640001
    [7] 7. The system of any one of claims 1 to 6, further comprising a de-polymerization reactor (70) for treating the first retentate (62) to provide a de-polymerized lignin stream (71).
    [8] 8. A method for treating spent pulping liquor (14) comprising lignin to providegreen liquor (47), the method comprising: (a) dividing the spent pulping liquor (14) into a first stream (18) and a secondstream (54); (b) evaporating (22) the first stream (18) to provide a concentrated pulping liquor(30); (c) incinerating (34) the concentrated pulping liquor (3 0) to provide a smelt (42); (d) filtering (58, 74) the second stream (54) to remove lignin, thereby obtaining aperrneate (66, 82) With reduced content of lignin; (e) dissolving (46) the smelt (42) in at least part of the perrneate (66, 82) toprovide green liquor (47).
    [9] 9. The method of claim 8, Wherein step (d) filtering (58, 74) the second stream(54) to obtain a perrneate (66, 82) comprises: (d1) filtering (58) the second stream (54) of the spent pulping liquor (14) toremove a first portion of lignin to provide a first retentate (62) and a first perrneate (66);and (d2) filtering the first perrneate (66) to remove a second portion of lignin toprovide a second retentate (78) and a second perrneate (82); Wherein at least part of the second perrneate (82) is used to dissolve the smelt (42) in the green liquor plant (46) in step (e).
    [10] 10. The method of claim 8 or claim 9, Wherein the second stream (54) is betweenabout 10 to 50% by volume of the spent pulping liquor (14), preferably about 25% byvolume of the spent pulping liquor (14).
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    同族专利:
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    引用文献:
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    法律状态:
    优先权:
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    SE1651205A|SE540646C2|2016-09-08|2016-09-08|Method and system for treating spent pulping liquor|SE1651205A| SE540646C2|2016-09-08|2016-09-08|Method and system for treating spent pulping liquor|
    JP2019512678A| JP2019533092A|2016-09-08|2017-09-05|Method and system for treating pulp effluent|
    US16/330,094| US20190249364A1|2016-09-08|2017-09-05|Method and system for treating spent pulping liquor|
    EP17772316.0A| EP3510195B1|2016-09-08|2017-09-05|Method and system for treating spent pulping liquor|
    PCT/EP2017/072204| WO2018046482A1|2016-09-08|2017-09-05|Method and system for treating spent pulping liquor|
    BR112019004387A| BR112019004387A2|2016-09-08|2017-09-05|system and method for treating residual pulping liquor.|
    CA3033451A| CA3033451A1|2016-09-08|2017-09-05|Method and system for treating spent pulping liquor|
    CN201780054995.1A| CN109689969A|2016-09-08|2017-09-05|For handling the method and system of pulping waste liquor|
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