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WO2024187276A1 - Procédé amélioré pour extraction de lignine kraft de liqueurs noires de bois dur et d'eucalyptus - Google Patents

Procédé amélioré pour extraction de lignine kraft de liqueurs noires de bois dur et d'eucalyptus Download PDF

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WO2024187276A1
WO2024187276A1 PCT/CA2024/050298 CA2024050298W WO2024187276A1 WO 2024187276 A1 WO2024187276 A1 WO 2024187276A1 CA 2024050298 W CA2024050298 W CA 2024050298W WO 2024187276 A1 WO2024187276 A1 WO 2024187276A1
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black liquor
lignin
black
liquor
factor
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Kurt WOYTIUK
George Sacciadis
Michael Paleologou
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FPInnovations
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FPInnovations
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for

Definitions

  • Softwood (SW), hardwood (HW) and eucalyptus (EW) wood species are pulped in conventional kraft processes globally and the latter is fast becoming the dominant market pulp due to the relatively fast growth rate of EW plantations and the uniformity of the pulp produced.
  • Three processes have been used commercially for the production of kraft lignin from black liquor, namely: LignoForceTM, LignoBoost and the Westvaco processes (Kienberger et al., Systematic review on isolation processes for technical lignins, Processes, 9, 804-822 (2021 ), the content of which is incorporated by reference).
  • kraft black liquor is acidified with carbon dioxide to a pH of about 10 at which pH lignin comes out of solution to form a lignin slurry.
  • the slurry is filtered in an effort to separate the lignin particles from the residual black liquor.
  • the lignin cake is then washed in place using dilute sulphuric acid and water or immersed in a dilute sulphuric acid solution to produce purified lignin in the acid form.
  • lignin is separated from the precipitated black liquor slurry, using a batch or continuous horizontal or vertical filter under pressure or vacuum. All commercial processes utilize such filters to separate and wash kraft lignin.
  • the flow rate through the porous filter media in the filtration system impacts primarily the initial few seconds while the lignin cake is formed and, subsequently, the filtrate and wash flow rate through the cake itself becomes rate limiting.
  • the separation of lignin from black liquor filtrate is, therefore, dependent on the properties of lignin particles and their interactions in forming lignin agglomerates. Filtration area is consistently the bottleneck in commercial lignin extraction processes due to the relatively high capital cost and complexity of filtration technologies. As a result, commercial production of kraft lignin is not economical when filtration area exceeds a certain design threshold.
  • HW and EW black liquors have been shown to have a more variable composition and processing behaviour compared to SW black liquors.
  • HW and EW lignin particles are often slow to filter in conventional industrial filtration equipment (belt, vertical, or horizontal tray filters) (please see, Tomani et al., Integration of lignin removal into a kraft pulp mill and use of lignin as a biofuel, Proceedings of the 5 th International Colloquium on Eucalyptus Pulp, Porto Seguro, Bahia, Brazil, May 9-12, 2011 ).
  • the lignin slurry in the case of HW and EW black liquors typically requires more than twice the filtration area to produce an equivalent mass of lignin to that of a SW lignin slurry.
  • some of these kraft lignin slurries have been observed to be completely unalterable using the conventional lignin slurry filtration processes. In fact, to avoid this problem, some researchers chose to use centrifugation to separate the lignin from the residual black liquor.
  • the lignin polymers in black liquor are comprised of syringyl, guaiacyl and p-hydroxyphenyl monomers.
  • the black liquor comprises free residual hemicelluloses and lignin-carbohydrate complexes (LCC).
  • the black liquor is a hardwood (HW) black liquor or a eucalyptus (EW) wood black liquor.
  • the black liquor is heated at a temperature between 140 and 180 °C.
  • the black liquor is heated to achieve an overall H-factor between 1800 and 2400, the cumulative H-factor being the sum of the H-factor at which the lignin in wood chips was subjected to in pulping plus the applied H-factor on the residual pulping liquor.
  • the REA level of the black liquor is firstly adjusted to a level of about 2.8-5 wt% Na 2 O on a black liquor solids basis prior to the heat treatment, preferably by adding for example sodium hydroxide.
  • the REA level of the black liquor is adjusted by adding white liquor.
  • the white liquor is partially oxidized white liquor or fully oxidized white liquor.
  • the black liquor with increased filterability is filterable through a belt, a vertical tray filter or a horizontal tray filter.
  • a process for removing lignin from HW, EW or soda black liquors comprising the steps of adjusting the minimum residual effective alkali (REA) level to about 2.8-5wt% Na 2 O on a black liquor solids basis; applying a heat treatment to said black liquor to achieve an overall H-factor of 1800-2400; acidifying the black liquor with an acidifier forming a lignin slurry; and filtering the lignin slurry to remove the lignin.
  • REA minimum residual effective alkali
  • the black liquor is acidified to a pH of about 10 forming a lignin slurry.
  • the black liquor is acidified to a pH of about 2-3 forming a lignin slurry.
  • the process for removing lignin from a black liquor as described herein further comprises the step of oxidizing with an oxidizing agent the black liquor before, after, or during the heat treatment step thus eliminating total reduced sulphur (TRS) compounds in the black liquor with oxidation of sulphides, mercaptans, and organic sulphides by said oxidising agent at a temperature effective for oxidation to thiosulphate- and other oxidized sulphur compounds and oxidation of said thiosulphate to sulphate, and such that hemicelluloses and other organics in the black liquor are oxidized by said oxidising agent at said temperature to form an acidifying agent selected from isosaccharinic acids, acetic acid, formic acid, lactic acid, oxalic acid, carbon dioxide and acidic lignin degradation products and mixtures
  • TRS total reduced sulphur
  • the oxidizing agent is oxygen
  • the acidifier is selected from carbon dioxide and sulphuric acid.
  • the acidifier is a strong acid such as for example sulphuric acid.
  • Fig. 1 illustrates the average specific filtration rates of lignin slurries derived from untreated HW (aspen) and SW (SPF) black liquors from the same swing mill processed at the demonstration plant level under similar conditions.
  • Fig. 2 illustrates a flowsheet of the process described herein in accordance to an embodiment in which the alkali addition and black liquor heat treatment steps precede the oxidation step of the LignoForceTM process.
  • Fig. 5 illustrates the average specific filtration rates of lignin slurries derived from the HW heat-treated black liquor from the mill of Example 1 at the laboratory level with no alkali addition.
  • Fig. 8 illustrates the average filtration rate of the slurry dewatering process in accordance to an embodiment, wherein an increase in filtration rate is consistent with pre- or post-oxidation heat treatments.
  • Fig 10 illustrates the average specific filtration rates of lignin slurries derived from heat-treated EW black liquor after adjusting the REA to 3wt% as Na 2 O and applying a heat treatment of 2000H (Mill 1 ) compared to SW black liquor (Mill 6, not heat-treated and no alkali added).
  • a process of increasing filterability of a lignin slurry derived from the acidification of HW and EW black liquors comprising the steps of adjusting the residual effective alkali (REA) level of said black liquor to about 2.8-5 wt%, preferably to about 2.8-3.8 wt%, as Na2O on a black liquor solids basis; and applying a heat treatment to said black liquor to achieve an overall H-factor of 1800-2400.
  • REA residual effective alkali
  • HW and EW black liquors are characterized by a lower molecular weight (MW) lignin of variable composition and morphology, and a higher carbohydrate content compared to SW black liquors.
  • the weight average molecular weight (M w ) of HW and EW kraft lignins is typically half that of SW kraft lignins resulting in lower relative viscosities after being dissolved in alkaline aqueous solutions or organic solvents.
  • the monomers of SW lignin are almost exclusively guaiacyl in nature whereas HW and EW lignins consist of both syringyl and guaiacyl units in variable ratios (S/G ratio).
  • HW kraft lignins also contain less condensed phenolics (i.e., less C-C linkages) and less crosslinking compared to SW kraft lignins.
  • the existence of free residual hemicelluloses (e.g., xylan) and hemicelluloses covalently bonded to HW and EW lignin reactive sites (in the form of so-called Lignin-carbohydrate complexes or LCC) in such black liquors is a major contributor to the variable filtration properties of HW and EW lignin slurries compared to SW lignin slurries for which the filtration properties are quite uniform.
  • lignin slurry filterability for black liquors collected from the same kraft pulp mill and precipitated at the demonstration plant level (50 kg/day) under similar conditions.
  • the lignin slurry filtration rate for this system in kilograms per hour per square meter of filtration area is measured as the total oven dry mass of lignin produced for each batch press divided by the cumulative pumping time for precipitated slurry sent to the press per square meter of filter area.
  • SPF a mixture of spruce, pine and fir usually referred to as SPF
  • 2020/0148835 applied a heat treatment at temperatures ranging from 150-250°C to softwood black liquor in the presence of added sodium hydroxide or white liquor and, optionally a capping agent and/or a solvent in an effort to depolymerize lignin in such black liquors before extraction using the LignoForceTM or other processes.
  • Nasman and Bjork, WO 2013/036190 applied a heat treatment to hardwood black liquor at a temperature above 160°C in an effort to precipitate out calcium compounds in the bulk of the black liquor thereby minimizing calcium carbonate scaling on evaporator surfaces and improving black liquor processability.
  • a peak temperature of between 140 and 180 °C and a heat treatment time of sufficient duration to provide overall H-factors (historical plus new) of 1800-2400 H were found to be most effective if a minimum level of Residual Effective Alkali (REA) content was present in the black liquors to be treated.
  • the heating and cooling exposure time were accounted for using the integral of the temperature-time curve (the area under the temperature-time curve in pulping is referred to as the H-factor as defined by Vroom (please see Vroom, K.E., Pulp Pap. Mag. Can., 58, 228 (1957).
  • applying H- factors between 800 and 1600 typically results in filtration rates equivalent to commercial softwood lignin recovery processes when the REA content in black liquor is sufficient for effective heat treatment.
  • the LignoForceTM process (please see US Patent No. 8,771,464, the content of which is incorporated by reference) was used to produce lignin from heat-treated HW and EW liquors at the laboratory and pilot plant levels. This process involves the following steps: a) Black liquor oxidation using oxygen; b) Black liquor acidification using carbon dioxide to a pH close to 10; c) Lignin slurry coagulation; d) Lignin slurry filtration to dewater the lignin cake; e) Lignin washing with dilute sulphuric acid; and f) Lignin washing with water.
  • Lignin slurry filterability is defined as the average rate of accumulation of filtrate up to 400 grams reported in kg / hr / m 2 of filtration area. Heat treatment time was varied to the extent needed to achieve the desired H-factors for applied black liquor heat treatment in consideration of the thermal history of any given black liquor.
  • FIG. 2 Three approaches were used successfully as described herein (see Figs. 2, 3, and 4). As shown in Fig. 2, the black liquor heat treatment step was applied ahead of the black liquor oxidation step while, as shown in Fig. 3, the black liquor heat treatment step was applied after the black liquor oxidation step. In Fig. 4, the black liquor heat treatment step was applied at the same time as the oxidation step.
  • a typical lignin recovery assembly comprises a weak black liquor tank 1 , a multiple effect evaporator (MEE) assembly 2, a black liquor oxidation reactor 3, a lignin precipitation reactor 4, a lignin coagulator 5 and a filter 6.
  • MEE multiple effect evaporator
  • Weak black liquor e.g. , 20% solids
  • the black liquor is heated in MEE assembly 2 to generate concentrated black liquor (e.g., 50% solids) which is directed to the mill recovery boiler along flow line 2b after being further concentrated (e.g. to 70-80% solids) in concentrators.
  • a side stream of black liquor is fed from assembly 2 (at about 30-40% solids) along flow line 2a to a mixing tank 7 where an alkali source 8 (such as but not limited to NaOH) is added.
  • the black liquor admixed with the alkali source is subsequently heated in the heater 9.
  • the heated black liquor admixed with the added alkali is then fed through line 9a to the black liquor oxidation reactor 3.
  • Oxygen gas is fed to the black liquor oxidation reactor 3 for oxidation of totally reduced sulphur (TRS) and other compounds in the black liquor.
  • TRS totally reduced sulphur
  • pre-treated black liquor is fed along flow line 3a to a lignin precipitation reactor 4, and CO 2 is fed as acidifying agent to the lignin reactor 4 to precipitate lignin in the liquor.
  • the oxidized black liquor can be further heated through line 3c before being fed along flow line 3a to the lignin precipitation reactor 4.
  • the acidified liquor is fed along flow line 4a to lignin coagulator 5 in which the precipitated lignin particles are allowed to coagulate.
  • Liquor with coagulated lignin is fed along flow line 5a to a filter 6 where lignin is filtered out of the liquor.
  • Lignin retained by filter 6 is optionally washed with H 2 SO 4 and water and washed lignin is recovered.
  • black liquor is fed from assembly 2 (at about 30-40% solids) along flow line 2a to the black liquor oxidation reactor 3.
  • the oxidized black liquor is then fed into a mixing tank where an alkali source 8 (such as but not limited to NaOH) is added.
  • the black liquor admixed with the alkali source is subsequently heated in the heater 9.
  • the heated black liquor admixed with the added alkali is then fed through line 3a to the lignin precipitation reactor 4.
  • black liquor is fed from assembly 2 (at about 30-40% solids) along flow line 2a to a mixing tank 7 where an alkali source 8 (such as but not limited to NaOH) is added.
  • the black liquor admixed with the alkali source is, subsequently, heated in the high temperature oxidizer 9 in the presence of oxygen.
  • the heated black liquor admixed with the added alkali is then fed to the lignin precipitation reactor 4.
  • the black liquor used resulted from the cooking of maple wood chips that were pulped at a Canadian kraft pulp mill under the following conditions:
  • Table 1 shows the composition of the HW black liquor obtained from the mill of Example 1 . It should be noted here that this liquor was not oxidized by the mill and it contained 4.24 wt% sulphide (on a black liquor solids (BLS basis)) as well as an REA of 2.87wt% on Na2O on a black liquor solids basis.
  • Fig. 5 shows the effect of applied H-factor on lignin slurry filtration rate. It should be noted that the filtration rate does not increase linearly or non-linearly with applied H- factor but displays a local maximum in filterability at approximately an applied H-factor of 1600 H. For the two trials exceeding 1600 H, the filterability is lower than the peak and equivalent to the filterability of the precipitated slurry treated at 900H.
  • the black liquor used resulted from the cooking of maple and birch wood chips that were pulped at a Canadian kraft pulp mill under the following conditions:
  • Wood type 50% maple and 50% birch
  • Fig. 6 shows the effect of increasing the effective alkali by adding NaOH to the black liquor prior to heat treatment at 2 levels of H-factor at the laboratory level.
  • the untreated black liquor with an REA content of 0.019 wt% (expressed as Na 2 O on a black liquor solid basis) and the black liquor with 2 wt% REA content have comparable filterability that is too low for future scale-up.
  • the filterability improved. The maximum filterability occurred at 5 wt% REA and 900H (applied H-factor).
  • the REA of the black liquor to be heat treated can be adjusted by either adding sodium hydroxide to the black liquor within the limits dictated by the caustic make-up requirements of the recovery cycle (usually 10 to 20 tonne/day in a typical 1000 tonne/d Canadian kraft mill).
  • a mill has the option of adjusting the REA of the black liquor to be heat-treated using cooking liquor (white liquor), partially oxidized white liquor or fully oxidized white liquor.
  • Partially oxidized white liquor is derived from white liquor whose sulphide content is mostly oxidized to thiosulphate while fully oxidized white liquor is derived from white liquor whose sulphide content is mostly oxidized to sulphate.
  • Fig. 7 shows the effect of the black liquor heat treatment as provided herein under different conditions on lignin MW.
  • the hardwood lignin weight average molar mass (Mw) is about 3000 g/mole as measured by gel permeation chromatography using an on-line refractive index (Rl) detector.
  • Mw weight average molar mass
  • Rl on-line refractive index
  • a control lignin slurry was derived from untreated aspen black liquor with the composition shown in T able 4.
  • the filtration rate of the control slurry was low but the dewatering process was successful and produced a reasonably good lignin cake with an ash content of 1 .2 wt% and a pH of 4.2.
  • a 2L Parr reactor was employed to evaluate the oxidation and heat treatment in a single process unit. Samples of HW black liquor were generated with either as-received residual effective alkali, or 4.9wt% effective alkali. The black liquors were then loaded into the reactor and heated to 90 °C.
  • Fig. 9 shows the filterability of the same HW black liquor discussed in Example 2 (produced from a mixture of birch and maple) at an adjusted REA content of 2.87 wt% as Na 2 O and after being heat-treated at two levels of H-Factor.
  • the filterability is defined here as the average filtration rate to recover 60% of the initial slurry mass reported in kilograms per hour per square meter of filter area.
  • the control lignin slurry (derived from untreated black liquor) of Example 5 was unalterable and, therefore, no lignin composition could be measured. Based on the black liquor composition shown in Table 5, NaOH solution was added to increase the REA to 3 wt% as Na2O on black liquor solids and the black liquor was heat treated to 2000H.
  • Fig. 10 compares the lignin slurry filtration rate of the heat-treated black liquor of Example 5 with the lignin slurry filtration rate of an untreated softwood black liquor with a low initial REA ( ⁇ 0.01 wt% as Na 2 O) at the pilot plant level. As shown in Fig.
  • T able 6 shows the composition of the lignin produced from the lignin slurry of the Example 5 heat-treated black liquor. It should be noted here that the ash content of this lignin is quite low as is the case with the lignins produced in Examples 1-4 from HW black liquors. The relatively high residual carbohydrate content of the lignin produced from the black liquor of Example 5 suggests that a somewhat more severe heat treatment would be required to achieve lower carbohydrate contents.
  • the black liquor pre-treatment approach of this patent disclosure does not only apply to difficult-to-filter HW and EW black liquors but also to difficult-to-filter black liquors derived from other pulping processes (e.g., soda process) as applied to wood or non-wood furnishes (e.g. wheat straw or bagasse straw).
  • Such liquors usually contain very high levels of hemicellulose (e.g., xylan) and lignin carbohydrate complexes (LCC) which, as discussed previously in this patent disclosure, are known to interfere with lignin cake dewatering and washing.
  • LCC lignin carbohydrate complexes
  • the black liquor acidification be conducted to a pH of 2-3 using sulphuric acid in order to maximize lignin yield.

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Abstract

L'invention concerne un procédé d'augmentation de la filtrabilité d'une pâte de lignine telle que celles dérivées de l'acidification de liqueurs noires de bois dur et d'eucalyptus, à un degré de filtrabilité comparable à des liqueurs noires de bois tendre. Le procédé d'augmentation de la filtrabilité d'une pâte de lignine telle que décrit ici comprend les étapes suivantes : l'ajustement de l'alcali effectif résiduel (AER) d'une liqueur noire de bois dur ou d'eucalyptus à un taux minimum d'environ 2,8 à 5 % en poids de Na2O sur la base des solides de la liqueur noire ; et l'application d'un traitement thermique à ladite liqueur noire pour obtenir un facteur H cumulé de 1800-2400 qui augmente la filtrabilité de la liqueur noire précipitée permettant la filtration dans des équipements de filtration industriels classiques tels que des filtres à bande, des filtres verticaux ou des filtres à plateaux horizontaux à des taux élevés.
PCT/CA2024/050298 2023-03-14 2024-03-12 Procédé amélioré pour extraction de lignine kraft de liqueurs noires de bois dur et d'eucalyptus Pending WO2024187276A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2976273A (en) * 1958-09-10 1961-03-21 West Virginia Pulp & Paper Co Treatment of kraft black liquor and product
WO2011150508A1 (fr) * 2010-06-03 2011-12-08 Fpinnovations Procédé pour la séparation de lignine d'une liqueur noire
WO2012005677A1 (fr) * 2010-07-07 2012-01-12 Stora Enso Oyj Procédé de production de lignine précipitée à partir de liqueur noire et lignine précipitée ainsi produite
WO2013178608A1 (fr) * 2012-05-28 2013-12-05 Södra Cell Ab Nouveau procédé et pâte dissolvante fabriquée par le procédé
WO2020013755A1 (fr) * 2018-07-13 2020-01-16 Södra Skogsägarna Ekonomisk Förening Procédé de séparation de la partie cellulosique d'une composition de polyester et de cellulose

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2976273A (en) * 1958-09-10 1961-03-21 West Virginia Pulp & Paper Co Treatment of kraft black liquor and product
WO2011150508A1 (fr) * 2010-06-03 2011-12-08 Fpinnovations Procédé pour la séparation de lignine d'une liqueur noire
WO2012005677A1 (fr) * 2010-07-07 2012-01-12 Stora Enso Oyj Procédé de production de lignine précipitée à partir de liqueur noire et lignine précipitée ainsi produite
WO2013178608A1 (fr) * 2012-05-28 2013-12-05 Södra Cell Ab Nouveau procédé et pâte dissolvante fabriquée par le procédé
WO2020013755A1 (fr) * 2018-07-13 2020-01-16 Södra Skogsägarna Ekonomisk Förening Procédé de séparation de la partie cellulosique d'une composition de polyester et de cellulose

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JARDIM JULIANA M., HART PETER W., LUCIA LUCIAN A., JAMEEL HASAN, CHANG HOU-MIN: "The Effect of the Kraft Pulping Process, Wood Species, and pH on Lignin Recovery from Black Liquor", FIBERS, MDPI AG, vol. 10, no. 2, 9 February 2022 (2022-02-09), pages 16, XP093213851, ISSN: 2079-6439, DOI: 10.3390/fib10020016 *
KIENBERGER MARLENE, MAITZ SILVIA, PICHLER THOMAS, DEMMELMAYER PAUL: "Systematic Review on Isolation Processes for Technical Lignin", PROCESSES, M D P I AG, CH, vol. 9, no. 5, CH , pages 804, XP093213848, ISSN: 2227-9717, DOI: 10.3390/pr9050804 *
WALLMO H., ET AL: "The influence of hemicelluloses during the precipitation of lignin in kraft black liquor", NORDIC PULP AND PAPER RESEARCH JOURNAL, vol. 24, no. 2, 1 February 2009 (2009-02-01), pages 165 - 171, XP055308954 *

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