US20150322104A1 - Method for producing high purity lignin - Google Patents

Method for producing high purity lignin Download PDF

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Publication number
US20150322104A1
US20150322104A1 US14/761,525 US201314761525A US2015322104A1 US 20150322104 A1 US20150322104 A1 US 20150322104A1 US 201314761525 A US201314761525 A US 201314761525A US 2015322104 A1 US2015322104 A1 US 2015322104A1
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Prior art keywords
lignin
content
carbohydrates
time period
reaction temperature
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Panu Tikka
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Valmet AB
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Valmet AB
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G1/00Lignin; Lignin derivatives
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00Regeneration of pulp liquors or effluent waste waters
    • D21C11/0007Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00Regeneration of pulp liquors or effluent waste waters
    • D21C11/0042Fractionating or concentration of spent liquors by special methods
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00Regeneration of pulp liquors or effluent waste waters
    • D21C11/04Regeneration of pulp liquors or effluent waste waters of alkali lye

Definitions

  • This invention relates to a method for producing high purity lignin, wherein lignin is separated from spent cooking liquor, called original black liquor, using a precipitation process.
  • the LignoBoostTM process was originally developed for production of an alternative bio-fuel, where main focus was at reduction of residual metal content, especially sodium, as the residual metal content may corrode boiler or burners using the lignin fuel. In this objective to reduce residual metal content it was shown that it was very important to maintain the process at the acidic side, and leaching and washing of lignin was kept at pH between 2-3 avoiding redeposition of metals, especially sodium, on the lignin.
  • An important aspect of the process is that the required charge of chemicals/acidifiers for the acidification and leaching of metals and subsequent washing may be high. If this is the case the cost of fresh chemicals is a large part of the operational cost and the commercial viability of the process is lower.
  • Another consideration is to minimize the acidic waste flows from the process as conventional recovery of spent chemicals may be impeded if volumes of acidic waste flows increase in relation to the alkaline bulk volume of black liquor being recovered.
  • Acidifiers in form of mill generated waste flows is thus preferable as it may both solve a waste disposal problem and lessen environmental impact as well as such usage would decrease costs for new chemicals.
  • the LignoBoostTM process produce a lignin product which if used as fuel is classified as a “green” fuel as being based upon recovered fuel.
  • the idea with classification of “green” fuels is based upon the concept not to increase the carbon dioxide footprint, i.e. the emissions, by burning fossil fuels.
  • the most promising acids for this process is carbon dioxide for at least initial precipitation of the lignin, and then using sulfuric acid (H 2 SO 4 ) for washing and leaching out metals from the lignin.
  • the sulfuric acid could be added as a fresh sulfuric acid from a chemical supplier, or as preferred using so called “spent acid” from a chlorine dioxide generator often used at a pulp mill.
  • so called “spent acid” from a chlorine dioxide generator often used at a pulp mill.
  • the latter usage of this spent acid already at hand in most mill sites further emphasize that the lignin product is considered as a “green” fuel.
  • U.S. Pat. No. 4,891,070 is disclosed a method for producing an improved aqueous printable ink composition from lignin. In this process extracting the lignin from the black liquor it is essential that the pH is not allowed to drop below pH 5 and adding an organic amine forming a lignin amine salt solution. In U.S. Pat. No. 4,891,070 is also disclosed other various methods of recovery, purification, and modification of lignin by-products as disclosed in U.S. Pat. Nos.
  • the original LignoBoostTM bio-fuel product produced a fuel with low residual levels of sodium and as it was used as a fuel no attention was drawn to the fact that the lignin fuel often had high levels of hemicelluloses, i.e. carbohydrates, as also hemicelluloses contributed to heat value of the fuel, even if the specific heat value of hemicelluloses is lower than pure lignin.
  • LignoBoostTM use black liquor from kraft pulping processes the hemicellulose content may vary considerably, and from worse case scenarios using cooking techniques like Lo-Solids Cooking could as much as 8-10% of the final lignin product correspond to hemicellulose/carbohydrate content.
  • lignin considered also for usage in production of spun fibers, used when producing light weight construction details in automobiles and airplanes. But in this process the lignin purity must be higher and residual levels of hemicelluloses must be very low, well below 1 wt-%. In other applications are lignin also considered for production of chemicals and in these processes is higher lignin purity also a requirement.
  • lignin is also known to decompose to solvable lignin if subjected to heat treatment at about 190° C. or higher, so the problem to reduce hem icelluloses content in a lignin product is not that obvious while maintaining the lignin yield high as well as reducing consumption of acidifiers and keeping acidic waste flows low.
  • a major concern when using the LignoBoostTM process has been the filterability of the lignin throughout the process, and heating of lignin is well known to cause softening of the lignin and that negatively affects filterability. So, solving the problem with carbohydrates in lignin is not that obvious as lignin yield should be kept high while carbohydrate content should be kept low.
  • the invention is based upon the surprising finding that an extensive hydrolysis of the lignin cake in the LignoBoostTM process could reduce the carbohydrate content in the lignin product considerably without any major losses in lignin produced.
  • the major part of the non soluble carbohydrate oligomeres are broken down to dissolvable monomers that easily could be separated from the lignin in the filtrate from a filtering stage subsequent to the hydrolysis.
  • the invention is related to a method for separation of lignin from original black liquor (BL IN ) having a first alkaline pH value, comprising the following stages in sequence:
  • the reaction temperature in the in the acidic slurry in the range of 100-120° C. and that the reaction time period during which at least 60% of the carbohydrates content is hydrolyzed is in the range 10-60 minutes in inverse proportion to temperature, keeping the amount of lignin dissolved from the lignin cake below 15%.
  • According to another embodiment of the invention is also a cooling effect introduced such that after the acidic slurry has been kept at the reaction temperature for a reaction time period during which at least 60% of the carbohydrates content is hydrolyzed, said acid slurry is subjected to cooling before subsequent separation of the treated lignin content.
  • the cooling effect is implemented such that the acidic slurry is cooled in an indirect heat exchanger against an acidifier to be used as the second acidifier, thereby reducing the temperature of the acidic slurry by at least 40° C.
  • the heat economy of the process will this be improved as the heat value from the hydrolysis liquid is transferred to the acidifier used for hydrolysis.
  • reaction temperature and time period corresponding to a P-factor equivalent to or exceeding the P-factor established at a reaction temperature of 100° C. and a time period of 60 minutes, i.e. a P-factor above 1.
  • the lignin cake subjected to an additional acidification to a pH of at least 2-4 or lower followed by a third separation of a third lignin cake as an additional treatment stage for leaching metals from said lignin cake, said additional treatment made either before or after obtaining the low carbohydrate lignin cake.
  • said additional treatment made either before or after obtaining the low carbohydrate lignin cake.
  • residual monosaccharide's be leached out from the lignin cake as well as residual metal content, as the acidic conditions in the leaching water is maintained avoiding redeposition of metals and/or monomers.
  • the lignin cake washed with washing water at a pH of at least 2-4 or lower after at least one of the separation stages.
  • separation stage embraces any means of separation.
  • the separation is performed by using centrifugation, a filter press apparatus, a band filter, a rotary filter, such as a drum filter, or a sedimentation tank, or similar equipment, most preferred a filter press apparatus is used.
  • original black liquor embraces spent cooking liquor from a digester, having most of the lignin from the original cellulose material dissolved in the “original black liquor”.
  • the “original black liquor” may also have a large content of organic and inorganic material, but may also have passed through separation processes for extracting turpentine or other specific constituents, while keeping the bulk volume of dissolved lignin unaltered.
  • FIG. 1 shows the basic steps in prior art lignin separation process according to WO 2006/031175
  • FIG. 2 shows the liquid balance established in last two stages when using a process shown in FIG. 1 ;
  • FIG. 3 shows content of the separated lignin using a process shown in FIG. 1 ;
  • FIG. 4 shows a principle modification of the process shown in FIG. 1 establishing a first alternative for the inventive method
  • FIG. 5 shows the liquid balance established in last two stages when using a process as shown in FIG. 4 ;
  • FIG. 6 shows a principle modification of the process shown in FIG. 1 establishing a second alternative for the inventive method
  • FIG. 7 shows the liquid balance established in last two stages when using a process as shown in FIG. 6 ;
  • FIG. 8 shows the content of the lignin material before and after using the inventive method at different hydrolysis conditions
  • FIG. 9 shows the residual carbohydrate content as a function of time and temperature
  • FIG. 10 shows how the hydrolysis results in purified lignin fraction and another fraction dissolved in the hydrolysis liquid.
  • LignoBoostTM process As a starting point for the invention was the LignoBoostTM process used, which is shown in principle in FIGS. 1 and 2 .
  • FIG. 1 is the process according to WO 2006/031175 shown.
  • the separation of lignin from original black liquor BL IN comprising the following stages in sequence:
  • the relatively small volume share of the lignin cake LIG 1 is the only volume needing further acidification for leaching of metals from the lignin, which means that the volumes of the second acidifier AC 2 is low in relation to original black liquor volumes.
  • the leaching process has been kept at operating conditions at pH 2-4 at 50-60° C. A lignin product could be produced at these conditions with very low residual content of sodium, thus suitable as a fuel in combustion plants.
  • FIG. 2 shows the liquid balance established in last two stages when using a process shown in FIG. 1 .
  • the FP 2 & DW stage shown as separated stages.
  • the first lignin filter cake LIG 1 is acidified using sulfuric acid, i.e. H 2 SO 4 .
  • FIG. 3 is shown the organic composition of the lignin cake obtained by using a process according to FIG. 2 , when treating an original black liquor obtained form a Soda-AQ cooking process with so called Lo-Solids cooking circulations during the cook.
  • Lo-Solids implies that black liquor is withdrawn in several positions during the cook and replaced with cooking liquor with low content of Dissolved Organic Material, i.e. DOM.
  • DOM Dissolved Organic Material
  • FIG. 4 a first preferred embodiment of the inventive method.
  • the new method steps as compared with the previous process shown in FIGS. 1 and 2 is the intensified acidification of the lignin cake LIG 1 and moderate heating of the acidified and reslurried lignin cake LIG 1 in the second acidification stage SS using a second acid or mixture of acids AC 2 .
  • the advantage with this embodiment is that no additional equipment is needed in comparison to the previous process as shown in FIG. 1 , besides additional heating and addition of more acidifier.
  • FIG. 5 shows the liquid balance established in last two stages when using the first preferred embodiment of the inventive method shown in FIG. 4 . In comparison with the liquid balance as disclosed in FIG.
  • FIG. 6 a second preferred embodiment of the inventive method.
  • the carbohydrates removed in an additional purification stage added after the process as shown in FIGS. 1 and 2 .
  • FIG. 7 shows the liquid balance established when using as additional purification stage according to the second preferred embodiment of the inventive method shown in FIG. 6 .
  • the amount of added sulfuric acid per ton of lignin precipitated increased from 200 kg from FIG. 2 up to 250 kg, i.e. a modest increase of about 25%.
  • the reasons for the modest increase of acidifier is that the intensified acidification to a pH of about 1.3 in last re-suspending and hydrolysis, compared to a pH of about 2-3 in preceeding stages, is that a large part of the acidic filtrate is returned from a subsequent filtration stage, i.e.
  • the first preferred embodiment results in reduced investment costs, if this is the primary objective, and the second preferred embodiment results in reduced operating costs as the charge of acidifiers is reduced considerably, and the second preferred embodiment is justified if available space is at hand at the mill for the extra equipment and the pay-off time is acceptable (cost for chemicals VS investment costs).
  • Carbohydrate removal was tested in laboratory using a 0.5 liter mechanically stirred reactor using lignin obtained from black liquor. 10-15 g of owen dry lignin suspended in 200 ml liquid was used in each test. The conditions for the carbohydrate hydrolysis tested was in the temperature range 80-120° C., at reaction time 10-60 minutes and at an established acidity of 0.5-4% H 2 SO 4 .
  • the constitution of the starting lignin material was as indicated in FIG. 8 . and several experiments were done, and results are plotted in FIG. 9 . What could be seen here is that all tests done at a hydrolysis temperature of 120° C. all achieved a residual level of carbohydrates under 1 wt-%.
  • the final result of the carbohydrate removal is shown in principle in FIG. 10 .
  • the initial lignin lost as dissolved carbohydrates and dissolved lignin in roughly about 50/50 proportions.
  • the purified lignin after the hydrolysis is then sufficiently clean for other purposes where residual carbohydrate content must be below 1-wt %, and the lignin fraction of the initial lignin suffers a yield loss below 10%.
  • the test examples was all conducted at a charge of H 2 SO 4 of 1.0 wt-%, which was found to be sufficient in order to establish a pH level of about 1.3 in the hydrolysis stage.

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Cited By (6)

* Cited by examiner, † Cited by third party
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CN104927067A (zh) * 2015-06-29 2015-09-23 南京林业大学 一种从竹材制浆黑液中提取不同分子量木质素的方法
US10072037B2 (en) * 2013-01-24 2018-09-11 Valmet Ab Method for producing high purity lignin
US20210060814A1 (en) * 2019-08-26 2021-03-04 Walker Industries Holdings Limited Aqueous wax emulsions and dispersions and uses thereof
CN114364841A (zh) * 2019-06-03 2022-04-15 苏扎诺有限公司 从黑液提取木质素的工艺
US11591472B2 (en) 2016-12-02 2023-02-28 The Williamette Valley Company Llc Wax-organic extender emulsion and method for manufacture thereof
WO2023083029A1 (zh) * 2021-11-10 2023-05-19 华南理工大学 一种绿色的碱木质素小分子分离方法及产物

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* Cited by examiner, † Cited by third party
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FI127125B (en) 2015-10-13 2017-11-30 Valmet Technologies Oy Process for the preparation of solid lignin
SE540485C2 (en) 2016-06-22 2018-09-25 Valmet Oy Method of producing lignin with reduced amount of odorous substances
SE540045C2 (en) * 2016-06-22 2018-03-06 Valmet Oy Method of producing lignin with reduced amount of odorous substances, lignin product obtained by the method and use of the lignin product
US20190241595A1 (en) * 2016-07-01 2019-08-08 Ren Fuel K2B Ab Ultrapure kraft lignin composition
WO2019241408A1 (en) * 2018-06-12 2019-12-19 Domtar Paper Company, Llc Methods and processes for lignin isolation/extraction
AT521179B1 (de) 2018-06-15 2019-11-15 Papierholz Austria Gmbh Verfahren zur Isolierung von Lignin aus einem alkalischen Prozessstrom
CA3160485A1 (en) 2019-12-06 2022-06-10 Basf Se Method for preparation of lignin oligomers
FI129507B (en) * 2019-12-20 2022-03-31 Andritz Oy Process for removing volatile compounds from a material containing lignin, use of a distillation process and material containing lignin
WO2022122575A1 (en) 2020-12-07 2022-06-16 Basf Se Aqueous lactam solution of lignin
AU2021405763A1 (en) 2020-12-23 2023-07-06 Basf Se Binder composition comprising polyamine(s) and hydroxyacetone for composite articles
AU2021405762A1 (en) 2020-12-23 2023-07-06 Basf Se Binder composition comprising polyamine(s) as well as 1,3 -dihydroxyacetone, glycolaldehyde and/or glyceraldehyde for composite articles
SE2150840A1 (en) * 2021-06-30 2022-12-31 Valmet Oy Method and system for lignin production
SE2150839A1 (en) 2021-06-30 2022-12-31 Valmet Oy Method and system for producing lignin
SE2250425A1 (en) * 2022-04-04 2023-10-05 Stora Enso Oyj Method for producing carbon from lignin
SE2250426A1 (en) * 2022-04-04 2023-10-05 Stora Enso Oyj Method for purifying lignin
SE545761C2 (en) * 2022-04-11 2024-01-02 Stora Enso Oyj A method for purifying lignin by removing inorganic impurities from black liquor

Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3817974A (en) * 1972-04-19 1974-06-18 Canadian Patents Dev Laundered amorphous reinforcing lignin
US4946946A (en) * 1988-10-17 1990-08-07 Imperial Chemical Industries Plc Production of low ash lignin
US20080047674A1 (en) * 2004-09-14 2008-02-28 Fredrik Ohman Method for Separating Lignin from Black Liquor
US20080051566A1 (en) * 2004-10-07 2008-02-28 Fredrik Ohman Method For Separating Lignin From A Lignin Containing Liquid/Slurry
US20080121356A1 (en) * 2006-11-27 2008-05-29 William Louis Griffith Method for improving separation of carbohydrates from wood pulping and wood or biomass hydrolysis liquors
US20080214796A1 (en) * 2004-09-14 2008-09-04 Per Tomani Method
US20100041879A1 (en) * 2006-12-22 2010-02-18 Lars Stigsson Method For Recovering A Low Sodium Content Lignin Fuel From Black Liquor
US20100325947A1 (en) * 2008-02-21 2010-12-30 Lignoboost Ab Method for separating lignin from black liquor, a lignin product, and use of a lignin product for the production of fuels or materials
US20110192560A1 (en) * 2008-10-21 2011-08-11 Danisco A/S Process of producing xylose and dissolving pulp
US20110294991A1 (en) * 2009-09-25 2011-12-01 Lake Michael A Process for recovering lignin
US20110297340A1 (en) * 2010-06-03 2011-12-08 Fpinnovations Method for separating lignin from black liquor
US20120196233A1 (en) * 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20130131326A1 (en) * 2010-07-07 2013-05-23 Stora Enso Oyj Process for production of precipitated lignin from black liquor and precipitated lignin produced by the process
US20130203972A1 (en) * 2010-10-15 2013-08-08 Upm-Kymmene Corporation Continuous method for the precipitation of lignin from black liquor
US20130331555A1 (en) * 2011-03-09 2013-12-12 Yrjö Mälkki Separation of lignin from plant material
US20140339455A1 (en) * 2011-12-09 2014-11-20 Upm-Kymmene Corporation Method for making a lignin component, a lignin component and its use and a product
US20150233057A1 (en) * 2014-02-18 2015-08-20 Api Intellectual Property Holdings, Llc Lignin-coated cellulose fibers from lignocellulosic biomass

Family Cites Families (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US113A (en) 1837-01-31 Improvement in the mode of making or preparing door-plates
US2680A (en) 1842-06-22 peters
US2525433A (en) 1947-09-23 1950-10-10 Huber Corp J M Inks
US2690973A (en) 1952-04-17 1954-10-05 Huber Corp J M Printing ink and varnish therefor
FR1112129A (fr) * 1953-11-19 1956-03-08 Inventa Ag Procédé pour la préparation de la lignine à partir des liqueurs noires
US3158520A (en) 1961-03-03 1964-11-24 Phillips Petroleum Co Method of sealing plastic film
US3094515A (en) 1961-11-06 1963-06-18 Lignosol Chemicals Ltd Lignin dispersing agents and a method of making the same
US3503762A (en) 1966-03-14 1970-03-31 Inca Inks Ink comprising lignin-based colorants
US3726850A (en) 1971-07-29 1973-04-10 American Can Co Lignin dispersing agent
US3769272A (en) 1972-05-25 1973-10-30 Westvaco Corp Lignin adduct
US3841887A (en) 1972-07-27 1974-10-15 Westvaco Corp Dyestuff compositions containing lignin surfactants carboxy substituted
US4184845A (en) 1975-04-18 1980-01-22 Westvaco Corporation Process for reduction of lignin color
US4001202A (en) 1975-10-17 1977-01-04 Westvaco Corporation Process for making sulfonated lignin surfactants
US4131564A (en) 1976-08-23 1978-12-26 Westvaco Corporation Lignin-containing dye dispersing composition
US4308203A (en) 1980-02-22 1981-12-29 American Can Company Sulfonated lignin dispersants and dyestuffs
US4355996A (en) 1980-03-24 1982-10-26 Westvaco Corporation Azo dye reduction improvement of lignin
US4891070A (en) 1987-04-13 1990-01-02 Westvaco Corporation Lignin amine salt as binder for aqueous printing ink composition
US20090176286A1 (en) * 2005-11-23 2009-07-09 O'connor Ryan P Process for Fractionating Lignocellulosic Biomass into Liquid and Solid Products
US8585863B2 (en) * 2007-09-21 2013-11-19 Api Intellectual Property Holdings, Llc Separation of lignin from hydrolyzate
US8608970B2 (en) 2010-07-23 2013-12-17 Red Shield Acquisition, LLC System and method for conditioning a hardwood pulp liquid hydrolysate
SE1150609A1 (sv) 2011-06-30 2012-12-31 Stora Enso Oyj Förfarande för rening av lignin
US20140065682A1 (en) * 2012-09-04 2014-03-06 Api Intellectual Property Holdings, Llc Processes and apparatus for producing fermentable sugars, cellulose solids, and lignin from lignocellulosic biomass
BR112015017598B1 (pt) * 2013-01-24 2021-05-18 Valmet Ab método para produção de lignina de alta pureza

Patent Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3817974A (en) * 1972-04-19 1974-06-18 Canadian Patents Dev Laundered amorphous reinforcing lignin
US4946946A (en) * 1988-10-17 1990-08-07 Imperial Chemical Industries Plc Production of low ash lignin
US20080047674A1 (en) * 2004-09-14 2008-02-28 Fredrik Ohman Method for Separating Lignin from Black Liquor
US20080214796A1 (en) * 2004-09-14 2008-09-04 Per Tomani Method
US20080051566A1 (en) * 2004-10-07 2008-02-28 Fredrik Ohman Method For Separating Lignin From A Lignin Containing Liquid/Slurry
US20080121356A1 (en) * 2006-11-27 2008-05-29 William Louis Griffith Method for improving separation of carbohydrates from wood pulping and wood or biomass hydrolysis liquors
US20100041879A1 (en) * 2006-12-22 2010-02-18 Lars Stigsson Method For Recovering A Low Sodium Content Lignin Fuel From Black Liquor
US20100325947A1 (en) * 2008-02-21 2010-12-30 Lignoboost Ab Method for separating lignin from black liquor, a lignin product, and use of a lignin product for the production of fuels or materials
US20110192560A1 (en) * 2008-10-21 2011-08-11 Danisco A/S Process of producing xylose and dissolving pulp
US20110294991A1 (en) * 2009-09-25 2011-12-01 Lake Michael A Process for recovering lignin
US20110297340A1 (en) * 2010-06-03 2011-12-08 Fpinnovations Method for separating lignin from black liquor
US20130131326A1 (en) * 2010-07-07 2013-05-23 Stora Enso Oyj Process for production of precipitated lignin from black liquor and precipitated lignin produced by the process
US20130203972A1 (en) * 2010-10-15 2013-08-08 Upm-Kymmene Corporation Continuous method for the precipitation of lignin from black liquor
US20120196233A1 (en) * 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20130331555A1 (en) * 2011-03-09 2013-12-12 Yrjö Mälkki Separation of lignin from plant material
US20140339455A1 (en) * 2011-12-09 2014-11-20 Upm-Kymmene Corporation Method for making a lignin component, a lignin component and its use and a product
US20150233057A1 (en) * 2014-02-18 2015-08-20 Api Intellectual Property Holdings, Llc Lignin-coated cellulose fibers from lignocellulosic biomass

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10072037B2 (en) * 2013-01-24 2018-09-11 Valmet Ab Method for producing high purity lignin
CN104927067A (zh) * 2015-06-29 2015-09-23 南京林业大学 一种从竹材制浆黑液中提取不同分子量木质素的方法
US11591472B2 (en) 2016-12-02 2023-02-28 The Williamette Valley Company Llc Wax-organic extender emulsion and method for manufacture thereof
CN114364841A (zh) * 2019-06-03 2022-04-15 苏扎诺有限公司 从黑液提取木质素的工艺
US20210060814A1 (en) * 2019-08-26 2021-03-04 Walker Industries Holdings Limited Aqueous wax emulsions and dispersions and uses thereof
US11752660B2 (en) * 2019-08-26 2023-09-12 Walker Industries Holdings Limited Aqueous wax emulsions and dispersions and uses thereof
WO2023083029A1 (zh) * 2021-11-10 2023-05-19 华南理工大学 一种绿色的碱木质素小分子分离方法及产物

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US10072037B2 (en) 2018-09-11
BR112015017598B1 (pt) 2021-05-18
EP2948590B1 (en) 2019-05-08
EP2948590A4 (en) 2016-08-17
CA2898449A1 (en) 2014-07-31
EP2948590A1 (en) 2015-12-02
WO2014116150A1 (en) 2014-07-31

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