US20150322104A1 - Method for producing high purity lignin - Google Patents
Method for producing high purity lignin Download PDFInfo
- 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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- United States
- Prior art keywords
- lignin
- content
- carbohydrates
- time period
- reaction temperature
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- Legal status (The legal status 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 status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- 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
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
- D21C11/0042—Fractionating or concentration of spent liquors by special methods
-
- 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
- D21C11/04—Regeneration 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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- Organic Chemistry (AREA)
- Paper (AREA)
- Compounds Of Unknown Constitution (AREA)
Applications Claiming Priority (1)
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PCT/SE2013/050051 WO2014116150A1 (en) | 2013-01-24 | 2013-01-24 | Method for producing high purity lignin |
Related Parent Applications (1)
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PCT/SE2013/050051 A-371-Of-International WO2014116150A1 (en) | 2013-01-24 | 2013-01-24 | Method for producing high purity lignin |
Related Child Applications (1)
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US15/648,661 Continuation-In-Part US10072037B2 (en) | 2013-01-24 | 2017-07-13 | Method for producing high purity lignin |
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US20150322104A1 true US20150322104A1 (en) | 2015-11-12 |
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US14/761,525 Abandoned US20150322104A1 (en) | 2013-01-24 | 2013-01-24 | Method for producing high purity lignin |
US15/648,661 Expired - Fee Related US10072037B2 (en) | 2013-01-24 | 2017-07-13 | Method for producing high purity lignin |
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US15/648,661 Expired - Fee Related US10072037B2 (en) | 2013-01-24 | 2017-07-13 | Method for producing high purity lignin |
Country Status (6)
Country | Link |
---|---|
US (2) | US20150322104A1 (pt) |
EP (1) | EP2948590B1 (pt) |
BR (1) | BR112015017598B1 (pt) |
CA (1) | CA2898449C (pt) |
PT (1) | PT2948590T (pt) |
WO (1) | WO2014116150A1 (pt) |
Cited By (6)
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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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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 |
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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)
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)
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 |
-
2013
- 2013-01-24 BR BR112015017598-8A patent/BR112015017598B1/pt active IP Right Grant
- 2013-01-24 CA CA2898449A patent/CA2898449C/en active Active
- 2013-01-24 EP EP13872956.1A patent/EP2948590B1/en active Active
- 2013-01-24 PT PT13872956T patent/PT2948590T/pt unknown
- 2013-01-24 US US14/761,525 patent/US20150322104A1/en not_active Abandoned
- 2013-01-24 WO PCT/SE2013/050051 patent/WO2014116150A1/en active Application Filing
-
2017
- 2017-07-13 US US15/648,661 patent/US10072037B2/en not_active Expired - Fee Related
Patent Citations (17)
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 |
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US20170355723A1 (en) | 2017-12-14 |
CA2898449C (en) | 2020-10-27 |
PT2948590T (pt) | 2019-07-12 |
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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