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WO2013036190A1 - Procédé pour le traitement de liqueur noire de bois de feuillus et liqueur noire de bois de feuillus traitée selon le procédé - Google Patents

Procédé pour le traitement de liqueur noire de bois de feuillus et liqueur noire de bois de feuillus traitée selon le procédé Download PDF

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Publication number
WO2013036190A1
WO2013036190A1 PCT/SE2012/050907 SE2012050907W WO2013036190A1 WO 2013036190 A1 WO2013036190 A1 WO 2013036190A1 SE 2012050907 W SE2012050907 W SE 2012050907W WO 2013036190 A1 WO2013036190 A1 WO 2013036190A1
Authority
WO
WIPO (PCT)
Prior art keywords
black liquor
hardwood
liquor
calcium
treatment
Prior art date
Application number
PCT/SE2012/050907
Other languages
English (en)
Inventor
Mats NÄSMAN
Maria BJÖRK
Original Assignee
Stora Enso Oyj
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 Stora Enso Oyj filed Critical Stora Enso Oyj
Priority to BR112014005055-4A priority Critical patent/BR112014005055B1/pt
Priority to EP12830388.0A priority patent/EP2753750B1/fr
Priority to ES12830388T priority patent/ES2729110T3/es
Priority to CN201280043097.3A priority patent/CN103842582A/zh
Publication of WO2013036190A1 publication Critical patent/WO2013036190A1/fr

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Classifications

    • 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
    • D21C11/10—Concentrating spent liquor by evaporation
    • D21C11/106—Prevention of incrustations on heating surfaces during the concentration, e.g. by elimination of the scale-forming substances contained in the liquors
    • 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
    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/08—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching

Definitions

  • the present invention relates to a process for treating a hardwood black liquor in order to prevent undesired fouling.
  • the present invention also relates to a hardwood black liquor treated according to the invention.
  • wood chips are treated in a digester system to separate the cellulose fibers and to remove desired amounts of lignin etc, which binds the fibers together in the natural state of wood, for the production of paper pulp.
  • Digestion of wood chips using an alkaline liquor is a common practice in the industry. In this process, commonly wood chips and an alkaline digesting liquor are introduced to a digester. After the digestions process the produced pulp and the digestion black liquor are separated to be further treated separately. The digestion black liquor at this point is withdrawn from the digester and then further treated in order to recover usable
  • the black liquor is evaporated to a higher dry matter content in a multi- stage evaporation plant in order to increase the efficiency of subsequent recovery steps.
  • a common problem in evaporation plants is fouling of the heat transfer surfaces which decreases the efficiency of the heat transfer. This leads to loss in productivity and higher operation costs. In order for the evaporation plants to run satisfactory the heat surfaces needs to be cleaned from time to time.
  • Calcium carbonate has been shown to be a key component of fouling on surfaces in the evaporation plant. Fouling tendency of calcium in cooking and/or black liquor has been shown to decrease dramatically after the liquor has been heated at or near typical full cooking temperatures. This action is, at times, referred to in the art as calcium deactivation by heat treatment.
  • An example of such calcium deactivation is described in EP 0313730 A1 which describes heating of cooking liquor high in calcium at or near full cooking temperature, holding it at this temperature in a vessel for a period of time, typically longer than ten minutes, and returning the heat treated liquor, with "deactivated" calcium, to a digester system.
  • Another object is of the present invention is to provide a black liquor with reduced fouling tendency.
  • the present invention relates to a process for treating a hardwood black liquor from the manufacturing of hardwood pulp in order to precipitate calcium ions present in the liquor wherein the process comprises the steps of; providing a hardwood black liquor from the manufacturing of hardwood pulp and treating at least one part of said liquor at a temperature of above 160°C wherein the calcium ions present in the black liquor will precipitate.
  • the hardwood used for the manufacturing of pulp is preferably eucalyptus, i.e. the black liquor is thus an eucalyptus black liquor.
  • eucalyptus black liquor comprises a large amount of free calcium ions, mainly due to the low cooking temperature but some eucalyptus species also comprises an increased amount of calcium. Consequently, the problem with undesired fouling is increased.
  • the hardwood is further preferably a plantation based wood.
  • the temperature during the treatment is preferably between 160- 190°C, more preferably above 165°C and also then preferred between 165- 185°C, and even more preferred between 170-180°C. Too low temperatures will not precipitate the calcium in a satisfactory way and too high
  • the treatment preferably lasts for less than 60 minutes, preferably below 40 minutes. The time needed depends on the black liquor being treated and on the temperature used.
  • the temperature is preferably increased by direct contact with a heating medium, preferably steam or vapor.
  • a heating medium preferably steam or vapor.
  • Suitable steam or vapor may be low-pressure fresh steam, medium-pressure fresh steam, high-pressure fresh steam or secondary vapor from the first evaporation stage.
  • the treatment is preferably done in a retention vessel, for example a separate vessel, a bottom part of an evaporator vessel or a separate section in an evaporation vessel. With this arrangement there will be no risk of fouling of heat surfaces in the evaporation vessel.
  • the heating medium may be added prior to the retention vessel, for example to a separate condenser located before the retention vessel or injected to a pipe located before the retention vessel. It is also possible to add the heating medium directly into the retention vessel.
  • the dry content of the black liquor to be treated is preferably between 30-45%.
  • the present invention further relates to a black hardwood liquor treated according to the process described above.
  • a black hardwood liquor treated according to the process described above By treating a hardwood black liquor at temperatures exceeding 160°C the calcium ions in the liquor will precipitate and form calcium carbonate crystals. It has also been shown that the viscosity of the treated hardwood black liquor is reduced at a given dry content which facilitates further treatment and handling.
  • the hardwood pulp is preferably hardwood kraft pulp. However, other pulps, such as pulps from sulfur free pulping processes may also be used.
  • the hardwood used for the manufacturing of hardwood pulp is preferably eucalyptus. It has been shown that eucalyptus black liquors comprise large amounts of calcium ions. It was found that temperatures exceeding 160°C is necessary in order for the free calcium ions to precipitate. However, black liquor from digestion of other hardwood species such as birch, aspen, acacia or poplar can also be treated according to the process of the invention.
  • the temperature during the treatment is increased to above 160°C. It is preferred that the temperature is between 160-190°C, more preferred above 165°C and thus also preferred between 165-185°C, more preferred between 170-180°C. Temperatures below or at 150°C have not been found to be able to precipitate any free calcium ions in a hardwood liquor in a satisfactory way. Too high temperature, e.g. temperatures above 190°C, is also not favorable since it requires a lot of energy to heat the liquor too much and it is thus not cost efficient. It is preferred that steam or vapor or a mixture of these is used in order to increase the temperature of the liquor.
  • Suitable steam or vapor may be low-pressure fresh steam, medium-pressure fresh steam, high-pressure fresh steam or secondary vapor from the first evaporation stage
  • Flashing will generate steam that can be re-used and thereby minimize overall energy consumption.
  • Cooling will generate warm water which could be of interest for instance for a mill producing district heating.
  • the treatment time is kept as short as possible. It has been shown that a time of less than 60 minutes is sufficient in order to precipitate the calcium ions in the form of calcium compounds, such as calcium carbonate, of the liquor. It is preferred that the treatment time is below 40 minutes, preferably between 5-30 minutes. The treatment may also last for less than about two hours. It is preferred that the treatment is done in a retention vessel for example a separate vessel, a bottom part of an evaporator vessel, a separate section in an evaporation vessel or in a separate condenser located before the retention vessel. The retention vessel does not comprise any heat transferring surfaces that the precipitated calcium can cause fouling on. The treatment is typically made before the second or the third effect in a seven stage counter-current evaporation plant. The purpose of the present invention is to make sure that the precipitation of calcium does not take place on e.g. the heat transferring surfaces of an evaporation vessel, i.e. to control the precipitation in order to prevent unwanted fouling.
  • the calcium will predominantly precipitate in the form of calcium carbonate. Once the calcium ions have precipitated they are no longer causing any problems with fouling and the precipitated calcium will continue together with the liquor to further treatment in the evaporation plant
  • the dry content of the hardwood black liquor to be treated is chosen so that it is not too high since calcium carbonate will precipitate at higher dry solid contents. If the dry content is increased to above the limit for
  • the hardwood black liquor to be treated according to the invention has a dry content of 30- 45%.
  • the deactivation process as set out above may be different depending on the different raw material used in the pulping process since the raw material may be different in chemical composition.
  • the required treatment temperature of the black liquor must though exceed the design cooking temperature but not be too high to negatively affect the energy balance of the mill.
  • Suitable liquor treating temperature range according to this invention is as set out above 160-190°C, and preferably 165-185°C.
  • eucalyptus was used as raw material but it is expected that similar results would be achieved with other hardwoods e.g. aspen, poplar, acacia and birch.
  • Preferred features of each aspect of the invention are as for each of the other aspects mutatis mutandis.
  • Black liquor from eucalyptus kraft cooking process was evaporated to 34.5 % dry solids content and treated at temperatures of 140°C, 170°C and 180°C for a period of 30 minutes.
  • Table 1 shows the results of measurement of soluble calcium in the black liquor after heat treatment according to the invention.
  • the calcium content was measured with inductively coupled plasma optical emission spectrometry (ICP-AES).
  • Table 1 Comparison of soluble calcium in untreated black liquor as reference and soluble calcium in black liquors treated for 30 minutes at different temperatures.
  • Black liquor treated 30 minutes at 180°C 460 A can be seen from Table 1 , the amount of soluble calcium is strongly reduced after a treatment at 180°C for period of 30 minutes. It can also be seen from Table 1 that the amount of soluble calcium is unaffected after treatment at 140°C for period of 30 minutes and that treatment at 170°C is able to reduce the amount of soluble calcium.
  • Black liquor from eucalyptus kraft cooking process was evaporated to 34.5 % dry solids content and treated at 180°C for periods of 5, 10, 20 and 30 minutes.
  • Table 2 shows the results of measurement of soluble calcium in the black liquor after heat treatment according to the invention.
  • the calcium content was measured with inductively coupled plasma optical emission spectrometry (ICP-AES).
  • Table 2 Comparison of soluble calcium in untreated black liquor as reference and soluble calcium in black liquors treated at 180°C for different periods of time.
  • the amount of soluble calcium is reduced after a treatment at 180°C.
  • the effective treatment time is leveling off after 20 minutes, i.e. it is not necessary to treat this eucalyptus black liquor for more than 20 minutes.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)

Abstract

L'invention porte sur un procédé pour le traitement d'une liqueur noire de bois de feuillus provenant de la fabrication de pâte de bois de feuillus afin de faire précipiter les composés du calcium présents dans la liqueur, le procédé comprenant les étapes consistant à : utiliser une liqueur noire de bois de feuillus provenant de la fabrication de pâte de bois de feuillus et traiter au moins une partie de ladite liqueur à une température au-dessus de 160°C, les composés du calcium présents dans la liqueur noire étant ainsi amenés à précipiter. L'invention porte également sur de la liqueur noire de bois de feuillus qui est traitée selon le procédé.
PCT/SE2012/050907 2011-09-05 2012-08-28 Procédé pour le traitement de liqueur noire de bois de feuillus et liqueur noire de bois de feuillus traitée selon le procédé WO2013036190A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BR112014005055-4A BR112014005055B1 (pt) 2011-09-05 2012-08-28 processo para o tratamento de licor negro de madeira de folhosa e licor negro de madeira de folhosa tratado de acordo com o processo
EP12830388.0A EP2753750B1 (fr) 2011-09-05 2012-08-28 Procédé pour le traitement de liqueur noire de bois de feuillus et liqueur noire de bois de feuillus traitée selon le procédé
ES12830388T ES2729110T3 (es) 2011-09-05 2012-08-28 Proceso para tratar el licor negro de madera dura y el licor negro de madera dura tratado de acuerdo con el proceso
CN201280043097.3A CN103842582A (zh) 2011-09-05 2012-08-28 处理硬木黑液的方法和根据这种方法处理的硬木黑液

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE1150800-9 2011-09-05
SE1150800 2011-09-05

Publications (1)

Publication Number Publication Date
WO2013036190A1 true WO2013036190A1 (fr) 2013-03-14

Family

ID=47832440

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE2012/050907 WO2013036190A1 (fr) 2011-09-05 2012-08-28 Procédé pour le traitement de liqueur noire de bois de feuillus et liqueur noire de bois de feuillus traitée selon le procédé

Country Status (6)

Country Link
EP (1) EP2753750B1 (fr)
CN (2) CN107503213A (fr)
BR (1) BR112014005055B1 (fr)
ES (1) ES2729110T3 (fr)
PT (1) PT2753750T (fr)
WO (1) WO2013036190A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4585746A1 (fr) 2024-01-15 2025-07-16 TSANDS Process Solutions, S.L. Procédé de récupération de composés à partir de cendres de chaudière kraft

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2063177A (en) * 1934-08-02 1936-12-08 Ralph H Mckee Recovery of organic constituents from black liquor
US3951753A (en) * 1969-06-03 1976-04-20 Roller Paul S Method and apparatus for the conversion of an aqueous scale-formed liquid
EP0313730A1 (fr) 1987-10-26 1989-05-03 Kamyr, Inc. Appareils et procédés pour réduire la formation de dépôts dans les processus de mise en pâte
WO1999002771A1 (fr) * 1997-07-11 1999-01-21 Sunds Defibrator Pori Oy Procede servant a traiter de la liqueur residuaire generee par la fabrication de pate a papier kraft
WO2000011263A1 (fr) 1998-08-21 2000-03-02 Andritz-Ahlstrom Oy Procede de prevention de l'incrustation
US6090240A (en) 1997-02-21 2000-07-18 Ahlstrom Machinery Oy Method of inhibiting scaling in black liquor evaporators

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IN154386B (fr) * 1979-12-10 1984-10-20 Dorr Oliver Inc
CN85106333A (zh) * 1985-08-19 1987-02-18 张沐恩 造纸黑液中碱和木质素的聚沉分离法
SE509444C2 (sv) * 1997-05-14 1999-01-25 Mo Och Domsjoe Ab Förfarande för minimering av kalcium orsakat inkrustproblem vid framställning av blekt cellulosamassa
SE9803384L (sv) * 1998-03-02 1999-09-03 Kemira Kemi Ab Förfarande för behandling av processvatten
GB0325578D0 (en) * 2003-11-03 2003-12-03 Bioregional Minimills Uk Ltd Method for treating black liquor
US7985318B2 (en) * 2007-05-10 2011-07-26 Nalco Company Method of monitoring and inhibiting scale deposition in pulp mill evaporators and concentrators

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2063177A (en) * 1934-08-02 1936-12-08 Ralph H Mckee Recovery of organic constituents from black liquor
US3951753A (en) * 1969-06-03 1976-04-20 Roller Paul S Method and apparatus for the conversion of an aqueous scale-formed liquid
EP0313730A1 (fr) 1987-10-26 1989-05-03 Kamyr, Inc. Appareils et procédés pour réduire la formation de dépôts dans les processus de mise en pâte
US6090240A (en) 1997-02-21 2000-07-18 Ahlstrom Machinery Oy Method of inhibiting scaling in black liquor evaporators
SE515452C2 (sv) * 1997-02-21 2001-08-06 Andritz Ahlstrom Oy Förfarande för förhindrande av beläggning av kalciumkarbonat i en indunstningsanläggning
WO1999002771A1 (fr) * 1997-07-11 1999-01-21 Sunds Defibrator Pori Oy Procede servant a traiter de la liqueur residuaire generee par la fabrication de pate a papier kraft
WO2000011263A1 (fr) 1998-08-21 2000-03-02 Andritz-Ahlstrom Oy Procede de prevention de l'incrustation

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
FREDERICK ET AL.: "Preventing Calcium Carbonate Scaling in Black Liquor Evaporators", PART TWO OF TWO, SOUTHERN PULP AND PAPER MANUFACTURER, August 1979 (1979-08-01), pages 22, 24, XP008174221 *
FREDERICK: "Preventing Calcium Carbonate Scaling in Black Liquor Evaporators", SOUTHERN PULP AND PAPER MANUFACTURER, September 1979 (1979-09-01), pages 22 - 29
See also references of EP2753750A4 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4585746A1 (fr) 2024-01-15 2025-07-16 TSANDS Process Solutions, S.L. Procédé de récupération de composés à partir de cendres de chaudière kraft
WO2025153507A1 (fr) 2024-01-15 2025-07-24 TSANDS Process Solutions, S.L. Procédé de récupération de composés à partir de cendres de chaudière kraft

Also Published As

Publication number Publication date
EP2753750B1 (fr) 2019-03-06
PT2753750T (pt) 2019-06-06
BR112014005055B1 (pt) 2021-01-12
CN107503213A (zh) 2017-12-22
BR112014005055A2 (pt) 2017-03-28
EP2753750A1 (fr) 2014-07-16
ES2729110T3 (es) 2019-10-30
CN103842582A (zh) 2014-06-04
EP2753750A4 (fr) 2015-04-22

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