WO2025043331A1 - Appareil et procédés d'extraction de lignine d'une liqueur noire non ligneuse - Google Patents

Appareil et procédés d'extraction de lignine d'une liqueur noire non ligneuse Download PDF

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Publication number
WO2025043331A1
WO2025043331A1 PCT/CA2024/051099 CA2024051099W WO2025043331A1 WO 2025043331 A1 WO2025043331 A1 WO 2025043331A1 CA 2024051099 W CA2024051099 W CA 2024051099W WO 2025043331 A1 WO2025043331 A1 WO 2025043331A1
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WIPO (PCT)
Prior art keywords
black liquor
wood
lignin
wood black
temperature
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Pending
Application number
PCT/CA2024/051099
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English (en)
Inventor
Douglas Mckenzie
Martin Pudlas
Michael Beattie
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Red Leaf Sustainable Ip Corp
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Red Leaf Sustainable Ip Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Red Leaf Sustainable Ip Corp filed Critical Red Leaf Sustainable Ip Corp
Priority to AU2024335178A priority Critical patent/AU2024335178A1/en
Priority to CN202480054661.4A priority patent/CN121773240A/zh
Publication of WO2025043331A1 publication Critical patent/WO2025043331A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • 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
    • 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
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials

Definitions

  • the present disclosure relates generally to lignin extraction, and more particularly to the extraction of lignin from non-wood black liquor.
  • Black liquor is a by-product of pulp production. It is a mixture of pulping residues, such as lignin and hemicellulose, and inorganic chemicals that are used to facilitate the pulping process.
  • black liquor may be combusted in a recovery boiler to extract energy from the pulping residues and to recover the inorganic chemicals for future use in the pulp production process.
  • the recovery boiler creates a bottleneck in the black liquor processing. In such cases, it may be desirable to pre-treat the black liquor to precipitate lignin therefrom prior to combustion to improve processing efficiency.
  • T raditional techniques for extracting lignin from wood-based black liquor may involve precipitation and filtering of the lignin from the wood-based black liquor.
  • the precipitated lignin can then be used as a valuable material for producing chemical products that reduce the use or generation of hazardous substances.
  • Lignin extraction reduces the thermal value of the remaining lignin-lean black liquor. The reduced thermal value creates a lower heat load on the recovery boiler, which can in turn be operated to process additional black liquor solids and support incremental pulp production.
  • Non-wood black liquor is a by-product of pulp production using non-wood feedstock such as straw.
  • Conventional lignin extraction processes for black liquor are not viable for non-wood black liquor due to the high silica and hemicellulose content in non-wood feedstock (e.g., wheat straw).
  • non-wood feedstock e.g., wheat straw.
  • studies have shown that existing commercial wood-based processes are ineffective on non-wood black liquor due to the poor filterability of the lignin in non-wood black liquor.
  • the elevated levels of silica present in non- wood black liquor will co-precipitate with the lignin, which impairs filtration and makes lignin removal difficult.
  • non-wood black liquor usually also contains high levels of hemicellulose, especially arabinoxylans, compared to conventional wood-based black liquor.
  • the elevated hemicellulose content can cause the formation of hydrogels which further impair the filterability and removal of precipitated lignin from solution.
  • the non-wood black liquor is oxygenated under pressure prior to cooling the non-wood black liquor.
  • the non-wood black liquor may be oxygenated under a pressure between 1 bar to 10 bar.
  • the non-wood black liquor may be oxygenated simultaneously with heating the non-wood black liquor to the first temperature.
  • the separated lignin is washed and the washed lignin is subsequently collected.
  • the lignin may be washed with hot water.
  • the non-wood black liquor is filtered using a filter press or a belt filter.
  • the non-wood black liquor is heated at the first temperature for a time period of between 5 minutes to 80 minutes.
  • the pH of the non-wood black liquor is chemically reduced to a value between 1 to 4 to precipitate out the lignin in the non-wood black liquor.
  • the pH of the non-wood black liquor may be chemically reduced by adding a mineral acid to the non-wood black liquor.
  • the non-wood black liquor is obtained from pulping non- wood feedstock that has been desilicated in a desilication process prior to pulping.
  • the non-wood black liquor may be cooled by indirectly preheating cooking chemicals used in the non-wood feedstock pulping process.
  • the desilication process may comprise mechanically separating silica from the non-wood feedstock with a mechanical pulper.
  • the desilication process may comprise chemically treating the non-wood feedstock with a chemical compound solution at a third temperature (e.g., between 50°C to 100°C) to selectively remove silica from the non-wood feedstock.
  • the chemical compound solution may comprise sodium carbonate, sodium hydroxide or potassium hydroxide.
  • the non-wood feedstock may comprise a straw-based feedstock.
  • FIG. 1 is a flowchart of a process for precipitating and extracting lignin from nonwood black liquor according to an example embodiment.
  • FIG. 2 is a flowchart of a supplementary process that can be adopted in conjunction with the FIG. 1 process to extract lignin from non-wood black liquor.
  • non-wood is used herein to refer to non-wood feedstock or agro-based fibers such as straw and/or agricultural residuals that remain after harvesting agricultural crops.
  • straw includes but is not limited to wheat straw, barley straw, oat straw, flax straw, rice straw, hemp, bamboo, miscanthus, sorghum, switchgrass, ryegrass, com stover, bagasse, reed stems and banana tree.
  • non-wood black liquor refers to the black liquor by-product produced from the process of manufacturing pulp from non-wood feedstock. As described in more detail elsewhere herein, non-wood black liquor usually has higher silica and hemicellulose content compared to wood-based black liquor, thereby making it more challenging to extract the lignin therefrom.
  • Process 10 utilizes a combination of chemical and mechanical means to precipitate, filter and separate lignin 15 from non-wood black liquor 17.
  • Process 10 utilizes a combination of chemical and mechanical means to precipitate, filter and separate lignin 15 from non-wood black liquor 17.
  • Dependent upon factors such as the composition of the non-wood feedstock and alkali addition rates, non-wood black liquor 17 collected from the pulping process may have a dissolved solids concentration that is typically in the range of 5% to 30%.
  • process 10 can extract lignin 15 from nonwood black liquor 17 having a dissolved solids concentration of less than 30%.
  • Process 10 begins with heating the non-wood black liquor 17 to an elevated temperature at heat treatment step 20.
  • the heat treatment of non-wood black liquor 17, even with elevated levels of silica contained therein, can improve the filterability of the precipitated lignin 15 downstream.
  • step 20 is performed to raise the temperature of non-wood black liquor 17 from, for example, room temperature (e.g., 20°C to 25°C) to between 150°C to 200°C.
  • the non-wood black liquor 17 is heated for a time period in the range of 5 to 80 minutes. Since hemicellulose is solubilized at temperatures greater than 150°C, raising the temperature of non-wood black liquor 17 can help enhance the degradation of the hemicellulose contained therein. It can be desirable to degrade the hemicellulose in the non-wood black liquor 17 early on in the process 10 (i.e. , at step 20) since hemicellulose content impairs the filterability and removal of precipitated lignin from solution.
  • process 10 After heating the non-wood black liquor 17 to a desired temperature for a desired period of time at heat treatment step 20, process 10 proceeds to optional oxygenation step 30.
  • the heated non-wood black liquor 17 is oxygenated under pressure to further enhance the filterability of the precipitated lignin downstream.
  • the oxygenation can help further degrade the hemicellulose remaining in the heated non-wood black liquor 17.
  • the oxygenation can also help reduce the pH of the heated non-wood black liquor 17 to thereby improve lignin colloid agglomeration.
  • the non-wood black liquor 17 may be oxygenated under pressure (e.g., between 1 bar to 10 bar).
  • oxygenation at step 30 also helps reduce the molecular weight of the organic acids in the non-wood black liquor 17 along with the biochemical oxygen demand (BOD) and chemical oxygen demand (COD) levels to improve the treatability of the lignin-lean filtrate 18 obtained downstream.
  • BOD biochemical oxygen demand
  • COD chemical oxygen demand
  • oxygenation step 30 may be performed before or simultaneously with heating step 20.
  • the oxygenation of the hemicellulose i.e., an exothermic process
  • process 10 proceeds to step 40.
  • the non-wood black liquor 17 is cooled to a temperature that is below the elevated temperature.
  • the non-wood black liquor 17 may be cooled to, for example, a temperature that is typically in the range of 65°C to 95°C.
  • the temperature is reduced at step 40 to facilitate the handling of the heat treated non-wood black liquor 17 in subsequent processing steps, but still usually maintained at a slightly elevated temperature (e.g., relative to room temperature) to encourage hemicellulose degradation.
  • the heat treated non-wood black liquor 17 is cooled by indirectly preheating cooking chemicals used in the non-wood feedstock pulping process. Cooling by indirectly preheating cooking chemicals improves the energy efficiency of the process.
  • process 10 After cooling the non-wood black liquor 17 to a desired temperature at step 40, process 10 proceeds to precipitation step 50.
  • the pH of the cooled non-wood black liquor 17 is reduced to precipitate out the lignin in the non-wood black liquor 17.
  • the pH of the non-wood black liquor 17 is reduced to a value between 1 to 4.
  • the pH of non-wood black liquor 17 is decreased in precipitation step 50 by adding a strong mineral acid, such as sulphuric acid, to the cooled non-wood black liquor 17.
  • a strong mineral acid such as sulphuric acid
  • Other acids such as nitric acid, phosphoric acid and hydrochloric acid can also be used in precipitation step 50.
  • step 50 requires only a strong acid (e.g., sulphuric acid), thereby reducing the chemical usage required for lignin precipitation.
  • a strong acid e.g., sulphuric acid
  • process 10 proceeds to filtration step 60.
  • filtration step 60 the lignin-lean filtrate 18 and the precipitated lignin 15 are separated to complete the lignin extraction process.
  • Filtration step 60 may be performed using a mechanical filter press, a mechanical belt filter, or the like. In contrast to existing lignin precipitation systems requiring the use of two or more filter presses for the separation and purification of the precipitated lignin, step 60 can be performed with the use of a single filter, thereby reducing the equipment required to separate and purify precipitated lignin.
  • Filtration step 60 may optionally comprise washing the extracted lignin 15.
  • the extracted lignin 15 may be washed using purified water and/or hot water.
  • the lignin-lean filtrate 18 obtained from process 10 has been effectively treated using aerobic treatment.
  • the lignin-lean filtrate 18 can also be treated anaerobically to produce a biogas.
  • FIG. 2 depicts an additional exemplary process 80 that can be implemented prior to process 10 to assist with lignin separation.
  • a desilication step 100 may be incorporated during the process of manufacturing pulp 92 from non-wood feedstock 90 to improve the filterability of the precipitated lignin in black liquor and to further enhance the efficiency of process 10.
  • silica can co-precipitate with lignin during precipitation step 50, thereby impairing filterability and the purity of the final lignin product.
  • non-wood feedstock 90 may be treated with hot water or a chemical solution (e.g., an alkaline solution) to pre-treat and separate some of the silica from the non-wood feedstock 90 during step 100.
  • the treatment may be conducted for a period of 10 to 30 minutes or more.
  • the non- wood feedstock 90 is heated and chemically desilicated with compounds like sodium carbonate, sodium hydroxide, potassium hydroxide, or the like.
  • Non-wood feedstock 90 may also be treated with hot water without the addition of alkaline chemicals in step 100.
  • the compounds used in desilication step 100 can preferentially separate silica (over, for example, lignin) from the non-wood feedstock 90.
  • desilication step 100 may be conducted under atmospheric pressure at temperatures in the range of 50°C to 100°C. If a strong alkali is used in step 100, then a relatively low reaction temperature (e.g., ⁇ 60 °C) may be sufficient to prioritize silica removal over delignification reactions. If a weak alkali or hot water is used in step 100, then a relatively high reaction temperature e.g., ⁇ 90 °C) may be required to prioritize silica removal over delignification reactions.
  • a relatively low reaction temperature e.g., ⁇ 60 °C
  • a relatively high reaction temperature e.g., ⁇ 90 °C
  • the non-wood feedstock 90 may be mechanically desilicated in step 100.
  • step 100 involves a combination of mechanical and chemical processes.
  • desilication step 100 may comprise mechanically pulping a stream of non-wood feedstock 90 after it has been heated and chemically reacted (e.g., in alkaline solution) to mechanically separate more silica from non-wood feedstock 90.
  • desilication step 100 Upon completion of desilication step 100, a relatively large amount of silica will be dissolved in the alkaline desilication liquor and selectively removed from the stream of non-wood feedstock 90.
  • the desilicated non-wood feedstock 90 may then be processed through a non-wood pulping process 200 to produce pulp 92.
  • the by-product non-wood black liquor 17 remaining from process 200 will have relatively low silica content.
  • Such non-wood black liquor 17 can then be processed using process 10 of FIG. 1 to extract lignin 15.

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Abstract

L'invention concerne des procédés, un appareil et des systèmes d'extraction de lignine d'une liqueur noire non ligneuse. La liqueur noire non ligneuse est chauffée à une première température pour dégrader l'hémicellulose contenue dans celle-ci. La liqueur est ensuite refroidie à une seconde température. Le pH de la liqueur refroidie est chimiquement réduit pour précipiter la lignine dans la liqueur. La liqueur est filtrée pour séparer la lignine précipitée de la liqueur.
PCT/CA2024/051099 2023-08-25 2024-08-23 Appareil et procédés d'extraction de lignine d'une liqueur noire non ligneuse Pending WO2025043331A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2024335178A AU2024335178A1 (en) 2023-08-25 2024-08-23 Apparatus and methods for extracting lignin from non-wood black liquor
CN202480054661.4A CN121773240A (zh) 2023-08-25 2024-08-23 用于从非木材黑液提取木质素的装置和方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US202363534666P 2023-08-25 2023-08-25
US63/534,666 2023-08-25

Publications (1)

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WO2025043331A1 true WO2025043331A1 (fr) 2025-03-06

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PCT/CA2024/051099 Pending WO2025043331A1 (fr) 2023-08-25 2024-08-23 Appareil et procédés d'extraction de lignine d'une liqueur noire non ligneuse

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CN (1) CN121773240A (fr)
AU (1) AU2024335178A1 (fr)
WO (1) WO2025043331A1 (fr)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004013409A1 (fr) * 2002-07-25 2004-02-12 Coffin World Water Systems Appareil et procede de traitement de liqueur noire
WO2006031175A1 (fr) * 2004-09-14 2006-03-23 Lignoboost Ab Methode pour separer de la lignine de liqueur residuaire
US20060225852A1 (en) * 2005-04-11 2006-10-12 Jan Pekarovic Process for removing silica from cellulosic material
US20100136642A1 (en) * 2006-05-08 2010-06-03 Biojoule Limited Recovery of lignin and water soluble sugars from plant materials
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
WO2012120184A2 (fr) * 2011-03-09 2012-09-13 Cerefi Ltd Séparation de la lignine d'une matière végétale
CA3193119A1 (fr) * 2020-08-27 2022-03-03 Mondi Ag Procede de separation de lignine a partir de liqueur noire

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004013409A1 (fr) * 2002-07-25 2004-02-12 Coffin World Water Systems Appareil et procede de traitement de liqueur noire
WO2006031175A1 (fr) * 2004-09-14 2006-03-23 Lignoboost Ab Methode pour separer de la lignine de liqueur residuaire
US20060225852A1 (en) * 2005-04-11 2006-10-12 Jan Pekarovic Process for removing silica from cellulosic material
US20100136642A1 (en) * 2006-05-08 2010-06-03 Biojoule Limited Recovery of lignin and water soluble sugars from plant materials
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
WO2012120184A2 (fr) * 2011-03-09 2012-09-13 Cerefi Ltd Séparation de la lignine d'une matière végétale
CA3193119A1 (fr) * 2020-08-27 2022-03-03 Mondi Ag Procede de separation de lignine a partir de liqueur noire

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CN121773240A (zh) 2026-03-31
AU2024335178A1 (en) 2026-04-09

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