WO2006037860A1 - Improved alkaline process and system for producing pulp - Google Patents

Improved alkaline process and system for producing pulp

Info

Publication number
WO2006037860A1
WO2006037860A1 PCT/FI2005/050346 FI2005050346W WO2006037860A1 WO 2006037860 A1 WO2006037860 A1 WO 2006037860A1 FI 2005050346 W FI2005050346 W FI 2005050346W WO 2006037860 A1 WO2006037860 A1 WO 2006037860A1
Authority
WO
WIPO (PCT)
Prior art keywords
impregnation
process according
liquor
cooking
stage
Prior art date
Application number
PCT/FI2005/050346
Other languages
English (en)
French (fr)
Inventor
Lasse Hernesniemi
Antti Tuominen
Tuomo NYKÄNEN
Rami Lampinen
Original Assignee
Metso Paper, Inc.
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 Metso Paper, Inc. filed Critical Metso Paper, Inc.
Priority to US11/663,976 priority Critical patent/US20070256801A1/en
Priority to CA002581923A priority patent/CA2581923A1/en
Priority to CN2005800416425A priority patent/CN101068977B/zh
Priority to EP20050795252 priority patent/EP1797235A4/en
Publication of WO2006037860A1 publication Critical patent/WO2006037860A1/en

Links

Classifications

    • 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
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/06Pretreatment of the finely-divided materials before digesting with alkaline reacting compounds
    • 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
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/02Pretreatment of the finely-divided materials before digesting with water or steam
    • 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
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/022Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing compounds
    • 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
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/22Other features of pulping processes
    • D21C3/222Use of compounds accelerating the pulping processes
    • 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
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/22Other features of pulping processes
    • D21C3/24Continuous processes

Definitions

  • the invention relates to an alkaline process for preparing pulp according to the preamble of claim 1 as well as a system for carrying out the process.
  • the objective of chemical pulping is to remove lignin so that the fibres can be separated with minor mechanical work.
  • alkaline cooking processes and especially kraft or sulfate cooking are dominant in the production of chemical cellulose pulp because they provide pulp fibers which are stronger than those obtained from other commercial pulping process.
  • the lignocellulosic material, typically cut into wood chips, is treated in either batch or continuous digesters with cooking liquor.
  • the active components of an aqueous solution of sulfate cooking liquor are hydroxide (OH) and hydrogen sulfide ions (HS).
  • OH hydroxide
  • HS hydrogen sulfide ions
  • the delignification takes place mainly by action of OH ions, but also the HS content in decisively significant in two ways: the hydrogen sulfide ions protect the carbohydrates of wood material whereby carbohydrate yield is improved, and on the other hand, they accelerate delignification reactions. Like the reactions of OH ions, also the rate of these reactions is increased with increased temperature.
  • anthraquinone In practice, it is not possible to cook high-quality cellulose using merely hydroxide, but catalytically acting anthraquinone (AQ) is additionally to be used. AQ may also be used in an ordinary kraft cooking, generally resulting in better yield and/or faster cooking. The yield can also be improved by a polysulfide treatment which has not shown to be easy to carry out in practice in industrial processes.
  • the use of anthraquinone is accociated with problems, as well: The use of AQ involves additional costs, and on the other hand, it cannot be used in all cellulose applications because of its toxicity. Pores inside fresh wood chips are partly filled with liquid and partly with a gas mixture consisting mainly of air.
  • the ratio is, among others, determined by the density, moisture and dry content of wood.
  • the air should be removed from the chips before they can be perfectly impregnated with cooking liquor. This is usually done by treating the chips with steam, and with respect of the present invention, for example, by using a process and a apparatus according to Finnish patent application FI 20021208.
  • Chip dimensions are of major importance in this context. The longer, wider and especially the thicker the chips are, the longer is the transportation distance to the central parts of the chips. If the transportation distance is too long and the rate of transportation too slow, the chemicals may be completely consumed before the cooking liquor can reach the chip centers, resulting in non-uniform cooking.
  • a commonly used measure for the time and temperature required for cooking reactions is the so-called Vroom H-factor expressing time integrale of the reaction rate as a function of time.
  • Vroom H-factor expressing time integrale of the reaction rate as a function of time.
  • a certain chip raw material can be understood to require, under constant conditions, an approximately constant H factor value.
  • a higher cooking temperature provides a required H factor value in a shorter time.
  • a low cooking temperature is an objective strived for, besides for the reasons of energy economy, also because of the yield and uniformity of the cook, but on the other hand, it means slower cooking reactions and thus a longer reaction time to obtain a certain H factor and a certain delignification degree. It leads naturally to larger digester volume, which, besides increasing investment costs, may at higher production levels cause problems in runnability of the process and thus in pulp quality.
  • the delignification reactions are generally divided to take place in three different steps: extraction delignification (1), bulk delignification (2) and residual delignification (3).
  • extraction delignification (1) the majority of the delignification reactions take place in step (2), and the reactions of step 3 are attempted to be avoided, because in that step cooking selectivity is essentially poorer than in step 2.
  • the delignification occuring during the step 1 is not selective, either, due to the fact that in this step many various reactions with chemical compounds of wood material take place.
  • Extraction delignification can be said to be based on the extraction of lignin bound to various carbohydrates, such as hemicellulose, from wood material. This, however, requires reactions with carbohydrates and thus a decrease in carbohydrate yield.
  • the chips are heated directly in a vapour phase and/or in several liquor heating circuits to a cooking temperature, and then typically cooked for at least 90 to 150 minutes in a concurrent and/or in a countercurrent cooking zone at temperatures below 165 0 C, in some overstressed digesters the maximum temperature may be even higher than that. Practical experience shows that the process becomes limited by chemical diffusion at cooking times of below about 90 to 150 minutes and temperature above 165 °C.
  • Typical cooking temperatures for softwood material are 145 - 165 °C, whereas for hardwood lower temperatures of 135 - 150 °C can be used, cf. e.g. international patent application WO 98/35091. Thus, a cooking time of about 90 - 150 minutes is required.
  • Contemporary continuous cooking processes as e.g. ITC, EMCC and Lo-solids cooking typically retain the cooking temperature through almost all of the aforesaid cooking zones, i.e. utilizing nearly the whole volume of the pressure vessel for cooking. These modern digesters have thus a total cooking zone of about 180 - 360 minutes.
  • washing filtrate is pumped into the bottom of the vessel.
  • a blow temperature is typically 85 - 95 °C.
  • the concentrations of the cooking liquor (dissolved dry matter, OH and HS ions) in a certain cooking stage are determined by the required amount of alkali, i.e. alkali consumption, the moisture of the chips and the dilution introduced with chemicals.
  • the HS ' ion content in white liquor being essential for the rate of the delignification reactions, is in fact high, but it cannot be added to exceed the amount of consumption in the cooking stage, resulting in spent liquor still containing a large amount of alkali, thus impacting the recovery of chemicals.
  • a too high OH concentration affects negatively the yield of the cooking.
  • the cooking liquor is considerably diluted by chip water. For this reason, it would be advantageous that the chips are as dry as possibly when entering the process. This is, however, not reasonable with respect to the quality nor the operability of the process, and it is not possible, either, to dry chips energy efficiently under control.
  • Patent application WO 03/062524 describes a method in which black liquor taken from cooking is evaporated before it is returned to the beginning of the cooking stage. From the end of the cooking stage the black liquor is intended to be fed to impregnation. The aim of this is to obtain a higher dry content which should improve cooking yield. The arrangement of this kind would also increase the absolute concentration of HS ions in the cooking stage. However, in several studies, it has been found that HS ions should be present already at the beginning of the whole extraction delignification and the bulk delignification to fully utilize the yield advantage and the increased rate of the cooking reactions obtained by them.
  • Swedish patent SE 521678 describes a method to increase sulfide concentration in impregnation in which method black liquour is taken from two different stages of the cooking and from which the latter can be, introduced to the impregnation through a expansion tank.
  • the independent claim states that the cooking temperature is in the range of 150 - 180 °C, and in connection with sulfide treatment the temperature should be at least 10 °C lower than the temperature of the cooking stage.
  • the method enables to increase the HS concentration to some extent in the impregnation and in the initial stage of the cooking, but the black liquor from the cooking stage cannot have a very high HS concentration without adding a relative great amount of alkali to the cooking stage since the majority of the consumption takes place in the impregnation stage. This would, in turn, lead to essentially decreased yield.
  • An objective of the present invention is to provide a process and a system which enable the use a temperature as high as possible in the impregnation of an alkaline cooking process so that carbohydrate yield after both the impregnation and the cooking stage can be maximized.
  • a process according to the invention is characterized by what is disclosed in the characterizing part of claim 1.
  • a system according to the invention is characterized by features disclosed in the characterizing part of claim 44.
  • the process according to the invention provides impregnation conditions enabling high concentrations of dissolved organic and inorganic dry matter of the impregnation liquor compared to those in the prior art.
  • the extraction delignification is carried out under optimal conditions as far as possible so that the extraction delignification would occur as little as possible or not at all in connection of the bulk delignification.
  • the system according to the invention enables to carry out the alkaline cooking according to the invention so that the liquid circulations of the impregnation stage and the cooking stages are separated from each other, and the impregnation liquor circulating in the impregnation stage can be concentrated.
  • the process according to the invention can be carried out in a continuous cooking process in a one- or two-digester cooking process, in a steam/liquid phase digester or in a hydraulic digester. Impregnation is performed either in an upper part of the digester or before the cooking stage or in a separate impregnation vessel.
  • the main principles of the process according to the invention are applicable also to a batch cook, especially a displacement batch cook.
  • the raw material can in principle be any lignocellulosic material. Different raw materials such as softwood, hardwood, bagasse and the like can be utilized in this process. Likewise, various end products such as bleached or unbleached pulp and a high- yield kraft pulp which optionally requires mechanical deliberation, can be produced by this process.
  • the black liquor from the cooking stage is not introduced to the impregnation in order to increase the level of the HS and of dry matter level which is a significant difference compared to prior art embodiments which utilize the HS/OH ion ratio of the black liquor generated in the cooking stage.
  • Liquid is transported to the cooking from the impregnation stage only inside the chips and in an amount carried during the transport of the chips..
  • the liquid-to-wood ratios of the impregnation stage and the cooking stage are separated from each other, the possibility to regulate the process in different stages is improved.
  • the liquids differ from each other as to their compositions and they contain reaction products from corresponding stages and cooking chemicals required for a stage.
  • impregnation liquor is meant an alkaline process liquor used in the impregnation stage.
  • cooking liquor is meant a liquor to be used in the bulk delignification, which liquor is removed from the digester or blown off together with pulp after the end of the cooking.
  • white liquor (WL), black liquor (BL) and green liquor have their common meanings used in sulfate processes.
  • fresh alkali an alkaline solution from the preparing system of chemicals, which in sulfate processes is white liquor or white liquor and green liquor.
  • the fresh alkali is mainly NaOH.
  • soda processes the fresh alkali corresponds to white liquor but it does not contain substantially sulfide.
  • Fresh alkali does not substantially contain dissolved organic dry matter.
  • Essential in the concept according to the invention is that free water is remover from the impregnation in stem form, e.g. by evaporation or by expansion, whereby high concentration differences required for diffusion maintain high.
  • the removal of water is effected partly or wholly in liquid form, e.g. by a membrane film.
  • the function of cations of the inorganic dry solid matter present in the impregnation liquor is to counteract the aforesaid Donnan effect, and the function of the organic matter is to buffer the impregnation liquor against yield losses of the chip material.
  • the level of the: inorganic and organic dry solid matter dissolved in the impregnation liquor is between 15 - 50%, preferably 20 - 35%.
  • the impregnation takes place by means of an alkaline impregnation liquor circulating in the impregnation stage to which fresh alkali is fed as an alkali addition and wherein the impregnation liquor is concentrated by removing water, e.g. by evaporating or by flashing, from it.
  • the process according to the invention is especially preferably sulfate cooking and the fresh alkali consists preferably essentially or entirely of white liquor.
  • alkali addition consists merely of fresh alkali or essentially merely of fresh alkali.
  • the alkali addition consists of fresh alkali and black liquor which is fed up to 1.0 ffiVodt.
  • the cooking process may also be soda cooking, whereby the fresh alkali consists of sodium hydroxide as dry or as a solution.
  • the fresh alkali addition fed to the impregnation liquor may consist of green liquor or green liquor and another fresh alkali, particularly white liquor.
  • the temperature is maintained as high as possible also in order to allow necessary degradations of the carbohydrates rapidly consume the hydroxide of the white liquor which will increase the HS-to-OH ratio.
  • the removal of water increases the hydrogen sulfide concentration to a high level.
  • the upper limit of the temperature is determined by the uniformity of the impregnation, the consumption of alkali and balances of the alkali as well as the starting of the bulk delignification.
  • the temperature of the extraction delignification in the impregnation stage is 135 ⁇ 55 0 C, preferably 135 ⁇ 20 °C, strongly depending on the raw material.
  • the temperature is 135 ⁇ 35 °C, preferably 135 ⁇ 10 °C It is also essential to carry out the extraction delignification stage as close to an end as possible so that this stage would not be carried out simultaneously with the bulk delignification or that extraction delignification would further occur as little as possible during bulk delignification.
  • the target yield by the impregnation is 80 ⁇ 15 %, preferably 80 ⁇ 10%, depending on the raw material to be used. In this the total yield after all delignification steps is maximized.
  • the impregnation may comprise several steps and consists preferably of one or two steps.
  • the first step a rise of the ratio of HS ions to OH ions is achieved towards the end of the step since the hydroxide is rapidly consumed at the beginning of the impregnation. In this way by a certain alkali amount it is possible to provide more reactive HS ions inside the chips.
  • the objective of the second step is to rapidly increase the alkali concentration before the bulk delignification which promotes uniform impregnation of the effective alkali to a chip, resulting in uniform cooking.
  • Essential in the impregnation is a high dynamic liquid- to-wood ratio, i.e. between the chips and the liquid phase there is a two to sevenfold, preferably a three to fivefold flow rate difference.
  • the extraction delignification is carried out as completely as possibly during the impregnation, particularly in the first step thereof.
  • the first step of the impregnation is carried out in a concurrent flow, and the second step of the impregnation may be concurrent or countercurrent.
  • the impregnation stage is merely concurrent.
  • the impregnation stage is merely countercurrent.
  • the amount of the effective alkali does not exceed 1.5 mol/1 NaOH, is preferably 0.5 - 1.5 mol/1 NaOH, particularly 0.8 - 1.2 mol/1 NaOH, preferably neither during the impregnation steps.
  • a rapid rise of the alkali concentration in the second step of the impregnation may be carried out at the beginning of the cooking stage before the bulk delignification begins, when the temperature of the cooking stage is low, preferably 140 ⁇ 10 - 0 C.
  • the amount of the alkali required for the bulk delignification is small compared to the total consumption, particularly when using hardwood.
  • due to the effective impregnation and hydrogen sulfide treatment after the temperature rise in the cooking stage the process proceeds directly to bulk delignification which bulk delignification is rapid.
  • the impregnation comprises a first step and a second step, whereby in the second step the OH concentration and the HS concentration are essentially higher than the corresponding concentrations at the end of the first step.
  • the HS concentration in the second step of the impregnation is essentially higher than at the end of the first step.
  • the OH concentration in the second step is essentially higher than at the end of the first step.
  • the alkaline cooking process according to the present invention for preparing pulp from lignocellulosic raw material comprises the impregnation of the raw material and the cooking of the impregnated raw material with cooking liquor. In an embodiment the raw material is steamed before its impregnation.
  • the concentration of the impregnation liquour is effected by heat energy from the cooking stage.
  • the concentration of the impregnation liquor is effected partly by means of heat energy brought from the cooking stage, whereby additionally other energy is used.
  • other energy than secondary energy from the cooking stage is used, e.g. low pressure steam or electric energy, e.g. by means of a compressor.
  • water is evaporated from the impregnation liquor by heating the impregnation liquor first indirectly by steam and by evaporating, and after that, the impregnation liquor is heated indirectly by means of the black liquor from the cooking stage to an impregnation temperature.
  • no energy is introduced to the process from the outside after the impregnation stage to elevate the temperature.
  • the majority of the alkali to be added to the raw material is added preferably to the steps of the impregnation.
  • the cooking stage of the -process according to the invention may preferably comprise both a concurrent and a countercurrent zone, whose alkali concentrations and temperatures can be regulated.
  • the cooking reactions of the process according to the invention can be terminated in the digester e.g. by displacing the cooking liquor or by diluting using filtrate from a wash plant, whereby the blow is carried out at a temperature below 100 °C.
  • the pulp is blown out essentially at a temperature higher than 100 0 C, optionally into a blow tank provided with heat recovery.
  • the pulp is blown out through a mechanical defibering stage into a blow tank.
  • Pulp was cooked under prior art conditions from eucalyptus chips in a laboratory, whereby the temperature in the first step of the impregnation was 110 0 C (duration 45 min) and in the second step 12O 0 C (15 min). The cooking temperature was kept at 152 °C for 120 minutes to obtain cellulose pulp having kappa number 17, which expresses the degree of delignification of the cellulose pulp. The liquors used were typical as to their HS and dry solid contents. The H factor expressing the ratio of the temperature to the cooking time was about 460. Pulp yield from the chips was 53.7% on the wood amount used.
  • the durations of the impregnation as in Example 1 were approximately double compared to those, of the cooking of example 1.
  • Nearly the same degree of delignification wasiobtained at a temperature of 149 0 C in a time of 100 minutes which means a H factor of 230 which is half of that of example 1.
  • Cellulose pulp yield was 54.5% on the wood amount used.
  • Figure 1 shows a preferred embodiment of the invention schematically.
  • Figure 2 shows a preferred embodiment of the invention with a separate impregnation vessel.
  • Figure 3 shows a preferred embodiment of the invention where impregnation and cooking are performed in the same vessel.
  • the arrangement according to the invention can be carried out e.g. according to fig. 1, wherein in chip treatment (1) the chips are treated with steam, which may be fresh or generated by flashing the liquor, to heat the chips and to remove air (gas mixture) from the chips. After that, a chips-liquor mixture with impregnation liquor is formed which mixture is introduced to impregnation (2).
  • the impregnation (2) comprises one, two or more steps having different chemical and/or temperature profiles.
  • the first step is carried out preferably in a concurrent flow, and the second step, depending on the case, in a concurrent or countercurrent flow.
  • the duration of the first step of the impregnation (2) is 15 - 120 minutes, preferably 15 - 45 minutes, and that of the second step of the impregnation is 5 — 60 minutes, preferably 10 - 45 minutes.
  • Liquor (BL) can be removed at the beginning of the impregnation steps (2), between the impregnation steps or before the cooking stage (3) e.g. by means of a screen zone or a screen/screw arrangement.
  • EL removed liquor
  • fresh alkali (white liquor) can be added, it can be heated directly or indirectly (8) and be introduced to expansion and/or evaporation (9).
  • the cooled liquor (IL) can be introduced into a level tank (10) for stabilizing flow variations. Separation of extractives and soap can also be carried out in the tank. Too much alkali (white liquor) should not be added to the liquors (BL) of the impregnation stage to avoid additional yield losses.
  • the hydroxide peak caused by the white liquor addition is diluted by a high dynamic liquid-to-wood ratio, i.e. by circulating free liquid.
  • This dynamic liquid-to-wood ratio may be 2 - 10 m 3 /Odt wood, preferably 3 - 6 m 3 /Odt.
  • the black liquor e.g. from the cooking stage
  • the impregnation liquor e.g. reject from fiber separation, 0 - 1.0 m 3 /Odt wood, preferably below 0.5 m 3 /Odt.
  • the removal of water (here evaporation) contained in the liquors (IL) of the impregnation stage (2) may be carried out e.g. in an expansion tank and/or in an evaporation unit (9), in one or more steps. Subsequent to that, the concentrated liquor flow may be heated to a desired temperature in one or more heat exchangers (11) wherein the heating flow may be e.g. steam, black liquor from the expansion screens of the digester or another secondary energy generated in the process or a combination thereof. This liquor (EL) to be circulated is returned to the impregnation stage at one or more points.
  • the concentrated liquor flow may be heated to a desired temperature in one or more heat exchangers (11) wherein the heating flow may be e.g. steam, black liquor from the expansion screens of the digester or another secondary energy generated in the process or a combination thereof.
  • This liquor (EL) to be circulated is returned to the impregnation stage at one or more points.
  • cooking liquor CL may be introduced which may consist of black liquor circulated from the end of the cooking and fresh alkali, here white liquor, optionally added thereto.
  • the amount of the circulated black liquor depends on a desired dynamic liquid-to-wood ratio in the cooking stage (3).
  • the dynamic liquid-to-wood ratio in the cooking stage (3) may be e.g. 2 - 6 mVODt (oven dry), preferably 3 - 4 m 3 /0Dt.
  • the corresponding values are 1-5 m 3 /0Dt, preferably 2-3 mVODt.
  • the temperature is maintained at 150 ⁇ 20 0 C for a sufficient time to obtain the required H factor.
  • the black liquor remaining at the end of the cooking stage (3) is first cooled by one or more heat exchangers (11), wherein the impregnation liquor is intended to be heated, and after that by one or more heat exchangers using cold water, if required.
  • the cooled black liquor is introduced to recovery (5-7) of cooking chemicals.
  • the pulp is cooled and transferred to washing (4).
  • the recovery (5 - 7) of cooking chemicals consists of evaporation units wherein black liquor (BL) is evaporated to raise its dry solid content to a level of 65 - 85 %.
  • black liquor (BL) is evaporated to raise its dry solid content to a level of 65 - 85 %.
  • a part of the evaporation work is carried out preferably in a water removal unit (9) in connection with the impregnation (2), whereby a number of the evaporation units (5) needed for the concentration of the black liquor can be correspondingly smaller.
  • the dry solid level of the feed liquor (BL) from the cooking stage (3) is higher than that in a cooking plant, where the evaporation is not carried out in connection with the impregnation (2), so-called feed liquor strengthening is not necessarily required in the evaporation plant (5), resulting in an increase of the capacity of the evaporation plant (5) and in improved energy economy.
  • the water removal unit (9) e.g. an evaporation unit
  • the recovery (5 - 7) e.g. in a process modification to the embodiment according to the invention.
  • the flow to be evaporated (IL) is still separated from other evaporation units (5) which evaporate black liquor (BL).
  • a superconcentrator (6) may be used before the black liquor is burnt in a soda recovery boiler (7).
  • a melt is formed which is dissolved to green liquor to obtain white liquor by causticizing (not shown in the figure).
  • the process according to the invention can be carried out in a continuous process or batch cooking process, especially in a displacement batch cook.
  • a preferred embodiment of the invention in a batch cook comprises a step before the impregnation stage in which chips are treated with steam to heat the chips and to remove gases.
  • a separate impregnation vessel may be used from which a chips-liquor mixture is filled to digesters.
  • the process may, in principle, be performed in present apparatuses, by changing i.a. liquid circulations so that the liquid circulations of the impregnation stage and the cooking stage are essentially separated from each other.
  • the impregnation (2) may be carried out e.g. in a separate impregnation vessel or in the same vessel as the cooking stage (3), however prior to the bulk delignification.
  • FIG 2 is shown one preferred embodiment of the invention with a separate impregnation vessel.
  • a reference number in meant a pump.
  • the chipped fiber material is fed through a chip bin to a chip treatment vessel (20), where air is removed from the chips.
  • the said vessel (20) can be e.g. according to a heating, steaming and storage apparatus shown in the patent application FI 20040637.
  • the fiber material is slurried by means of a liquid flow (50) which in this case is impregnation liquor and the slurried fiber material (51) is fed to a chip feeder (21).
  • the chip feeder is a feeder with which material in slurry form can by transported from a first pressure system to a system having a second, higher pressure.
  • the impregnation is with two steps: before screens (Sl, S2) the impregnation is concurrent and after the screens countercurrent.
  • the slurried fiber material is fed by means of the chip feeder (21) along line 52 to a continuous impregnation vessel (22).
  • Impregnation liquor used for the transportation of the chips is separated from the chips in the upper part of the impregnation vessel by means of equipment known in the art.
  • Transportation liquid (53) is returned by means of the chip feeder apparatus (21) to the evaporation circulation where impregnation liquor is concentrated.
  • the pressure screen (23) can alternatively be replaced with a tube screen known in the art.
  • Fresh alkali here white Ii quor WL
  • the impregnation liquor is heated in a heat exchanger (24) whereto low pressure steam (57) is fed.
  • the heated liquor flow is directed to a water removal unit 25 along line 84.
  • the impregnation liquor is concentrated by removing water from it.
  • Part of the steam (58) exiting the water removal unit 25 is directed along lines 59, 60 and 61 to be used in chip heating and pre-steaming, and part of it is removed wholly from the impregnation circulation and cooking circulation and is directed to the condenser.
  • the impregnation liquor may be concentrated further at the second water removal unit 26 and the steam generated is directed to condenser.
  • Water removal units 25 and 26 can be e.g. expansion tanks and/or evaporation units.
  • the impregnation liquor concentrated at water removal unit 25 is directed along line 85 to a water removal unit 26.
  • the concentrated impregnation liquor (62) is fed to a level tank (27).
  • soap is removed from the impregnation liquor in the level tank, after which impregnation liquor (63) is pumped (P5) to an impregnation vessel and if necessary, along line 50 for slurrying of the chips.
  • the surface level of the level tank is regulated by the magnitude of flow 63.
  • the impregnation liquor (63) fed to the impregnation vessel is heated in a heat exchanger (28) utilizing the heat of the black liquor (64) coming from the digester.
  • the heated liquor flow (65) is pumped (P4) through a heat exchanger (29) to the bottom of the impregnation vessel (22).
  • the impregnation liquor is combined with a liquor flow from the upper part of the digester, which liquor has been used to transport the impregnated fiber material from the impregnation vessel to the digester (30).
  • low pressure steam (66) directed thereto is used.
  • Impregnation liquor is removed from the impregnation vessel though screen S2 to line 68 and through a central tube screen along line 69 which joins line 68.
  • the impregnation liquor which is diluted by the water in chips, is removed through screen Sl and through the central tube screen and through line TO to line Tl wherefrom it is pumped to return circulation 53 and thereby returned to the water removal of the impregnation liquor.
  • Part of the flow Tl is directed directly to a heat exchanger 24 preceding the water removal unit 25 by means of line T2.
  • the impregnation liquor is directed through line 65' to the chip- impregnation liquor-flow (52) going to the first step of the impregnation vessel.
  • Steam generated at the first water removal unit 25 can be directed to chip steaming in the chip treatment vessel (20) and/or to the chip bin preceding it (not in the figure).
  • the impregnation liquor which is used in impregnation and is circulating in the impregnation, is concentrated when part of the steam generated in the water removal unit 25 and the steam (14) generated in the water removal unit 26 in its entirety, is removed from the whole system to the condenser, i.e. part of the steam is not returned to the chips.
  • Steam and air (83) from the chip treatment vessel (20) is removed to the condenser.
  • the impregnated fiber material is removed from the bottom of the impregnation vessel (22) and is transferred to a continuous digester (30) along line T3.
  • the embodiment according to figure 2 is a steam-liquid phase-digester. Impregnation liquor used for transportation of chips is removed from the top of the digester by means of equipment known in the prior art and the said impregnation liquor is returned along line T4 by means of pump P4, through a heat exchanger 29 to the bottom of the impregnation vessel (22).
  • the digester (30) is heated with low pressure steam or with middle pressure steam (81) which preferably originate from the power plant of the mill.
  • the dynamic liquid to wood- ratio in the upper part of the digester is regulated by pumping with pump PI l black liquor sucked from the central tube screen along line 75 to the upper part of the digester.
  • Fresh alkali here white liquor WL
  • Black liquor removed by central tube screens is added through line 16 to the black liquor flow leaving the digester through expansion screens S3 and S4.
  • Black liquor removed from the digester (30) through screens (S3, S4) and through central tube screens is used to heat at the heat exchanger (28) the impregnation liquor from the level tank to the impregnation vessel, after which the black liquor is directed to a pressure screen 31.
  • the accept stream of the pressure screen is directed to the chemical recovery and the reject (77) to washing filtrate (78) or to the stream (50) for slurrying the chips.
  • black liquor is removed through stream 79 and is circulated to screen S5.
  • White liquor (80) is added to this stream (79). Washing filtrate (78) is fed to the bottom of the digester (30) with pump P13.
  • FIG. 3 shows a preferred embodiment of the invention where impregnation and cooking are performed in the same vessel.
  • Chips are fed to the chip bin (100) wherefrom the heated chips are fed by means of a low pressure feeder (101) to a pre-steaming vessel (102) to remove air from the chips.
  • Chips are fed from the pre-steaming vessel (102) through a chip ' chute (103) to a chip feeder (104) by means of which the chips are fed to a digester (105) with a higher pressure.
  • the chip feeder (104) can be e.g. a high pressure feeder according to prior art.
  • Impregnation and cooking of the chips is performed in the digester (105).
  • P before a reference number refers to a pump. From the pre-steaming vessel (102) steam and air (108) can be removed and directed to a condenser.
  • the slurried fiber material is fed by means of the chip feeding apparatus (104) along line 150 to the digester (105). Impregnation liquor used for the transportation of the chips is separated from the chips in the upper part of the digester by means of equipment known in the art.
  • Transportation liquid (151) is returned by means of the chip feeder apparatus (104) to water removal where impregnation liquor is concentrated.
  • the impregnation liquor (152) exiting from the chip feeder (104) is pumped (P24) to a pressure screen (99) in order to remove fiber material, whereby the reject flow (182) obtained is guided back to the chip chute (103).
  • the pressure screen (99) can alternatively be replaced e.g. with a tube screen known in the prior art.
  • the accept flow (153) is heated in a heat exchanger (106) whereto fresh steam (154) is fed.
  • the heated impregnation liquor (155) is directed to the first water removal unit 107, where the impregnation liquor is concentrated by removing water from it. Part of the steam leaving from the water removal unit 107 is directed along line 156 to be used in chip pre- steaming (102) and the rest (157) is directed to a heat exchanger (109) to heat the impregnation liquor.
  • the impregnation liquor can be concentrated further at the second water removal unit (108) wherefrom the leaving steam (158, 159) is directed to a condenser and to chip bin (100) for heating and steaming the chips.
  • the water removal units (107, 108) can be e.g. expansion tanks and/or evaporation units.
  • the concentrated impregnation liquor (160) is directed to a level tank (110). From the line (160) impregnation liquor is returned to the water removal through line 161. In the line 161 fresh alkali (here white liquor WL) is added from line 162 to the impregnation liquor and the mixture is pumped with pump P25 to the heat exchanger 109 wherefrom it is directed ' to line 153.
  • fresh alkali here white liquor WL
  • soap is removed from the impregnation liquor which soap is removed along line 163 by means of pump P22.
  • the impregnation liquor (164) is pumped with a pump (P27) to impregnation.
  • Impregnation liquor 164 which is fed to the impregnation steps is heated in a heat exchanger (111) utilizing the heat of the black liquor (165) coming from the digester.
  • the impregnation is in two steps: before the first screen (S21) impregnation us concurrent and between the first (S21) and the second screen (S22) concurrent or countercurrent.
  • Impregnation liquor is removed from the first step of the impregnation through screen S21 to water removal (stream 178).
  • the concentrated impregnation liquor is returned to the first step of impregnation to the upper part of the digester (164) and to the second step of the impregnation along line 166 either to heating circulation 167 and/or 168.
  • line 166 either to heating circulation 167 and/or 168.
  • line 166 either to heating circulation 167 and/or 168.
  • Lines 167 and 168 include heat exchangers (not shown in the figure) working with fresh steam in order to heat the impregnation liquor.
  • the cooking step subsequent to the second screen S22 is concurrent.
  • Black liquor from the end of the cooking can be circulated from screen S23 by means of a pump P214 along line
  • the step between the screens S23 and S24 can be concurrent or countercurrent.
  • liquor is circulated along line 170 which is equipped with a heat exchanger, to which line fresh alkali (here white liquor) is added (line 174) before pump (P210).
  • Black liquor is removed from the digester along line 165.
  • cooking liquor is removed along line_170'.
  • the heat of the black liquor removed from the digester is utilized for heating of the white liquor in heat exchanger 111, after which the black liquor is directed to, via cooling and fiber separation (112, 113) to the chemical recovery along line 172.

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PCT/FI2005/050346 2004-10-04 2005-10-04 Improved alkaline process and system for producing pulp WO2006037860A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US11/663,976 US20070256801A1 (en) 2004-10-04 2005-10-04 Alkaline Process and System for Producing Pulp
CA002581923A CA2581923A1 (en) 2004-10-04 2005-10-04 Improved alkaline process and system for producing pulp
CN2005800416425A CN101068977B (zh) 2004-10-04 2005-10-04 用于生产纸浆的改进的方法和系统
EP20050795252 EP1797235A4 (en) 2004-10-04 2005-10-04 IMPROVED ALKALINE PROCESS AND SYSTEM FOR PRODUCING PAPER PULP

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20041288 2004-10-04
FI20041288A FI120547B (fi) 2004-10-04 2004-10-04 Alkalinen keittomenetelmä ja laitteisto massan valmistamiseksi

Publications (1)

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WO2006037860A1 true WO2006037860A1 (en) 2006-04-13

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PCT/FI2005/050346 WO2006037860A1 (en) 2004-10-04 2005-10-04 Improved alkaline process and system for producing pulp

Country Status (6)

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US (1) US20070256801A1 (fi)
EP (1) EP1797235A4 (fi)
CN (1) CN101068977B (fi)
CA (1) CA2581923A1 (fi)
FI (1) FI120547B (fi)
WO (1) WO2006037860A1 (fi)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2265759A1 (en) * 2006-11-07 2010-12-29 Metso Fiber Karlstad AB Method for an energy efficient production of cellulose pulp in a continuous digester
WO2011138633A1 (en) * 2010-05-04 2011-11-10 Bahia Specialty Cellulose Sa Method and system for pulp processing using cold caustic extraction with alkaline filtrate reuse
AU2008203206B2 (en) * 2007-08-07 2011-12-15 Andritz Inc. Method and System for Semi-Chemical Pulping
US8535480B2 (en) 2010-05-06 2013-09-17 Bahia Specialty Cellulose Sa Method and system for pulp processing using cold caustic extraction with alkaline filtrate reuse
EP3124693A1 (fr) * 2015-07-31 2017-02-01 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procede de traitement de la liqueur noire provenant de la preparation de pate a papier par liquefaction hydrothermale
EP3377696A4 (en) * 2015-11-16 2019-08-21 Valmet AB METHOD FOR HEATING CELLULOSE MATERIAL AT FULL COOKING TEMPERATURE IN CELLULOSE COOKERS

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI20090079A (fi) * 2009-03-05 2010-09-06 Andritz Inc Lämmön talteenotto jätekeittolipeästä sellutehtaan keittämöllä
US20100263813A1 (en) * 2009-04-21 2010-10-21 Andritz Inc. Green liquor pretreatment of lignocellulosic material
CN103924471B (zh) * 2014-04-02 2017-07-28 上海同化新材料科技有限公司 一种改性木质纤维素的制备及其产物
FI126802B (fi) * 2014-09-12 2017-05-31 Andritz Oy Menetelmä ja hydraulinen vuokeitinjärjestelmä kemiallisen massan tuottamiseksi
CN106381743B (zh) * 2016-11-19 2018-02-16 王芹 一种纤维精制工艺
CN108867131A (zh) * 2016-12-20 2018-11-23 常州爱上学教育科技有限公司 用于制浆造纸的木、竹原料节能环保置换蒸煮工艺
CN109957981A (zh) * 2017-12-25 2019-07-02 福建省青山纸业股份有限公司 一种生产高强高透伸性纸袋纸工艺方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3258390A (en) * 1962-10-20 1966-06-28 Domtar Ltd Method and apparatus for maintaining a water balance during impregnation and digestion of cellulosic material
US3448002A (en) * 1964-06-20 1969-06-03 Domtar Ltd Pulping process
US3802956A (en) * 1970-03-17 1974-04-09 Kamyr Ab Method for impregnation of cellulosic fiber material with digesting liquor while preventing dilution of said liquor
US3814662A (en) * 1969-09-08 1974-06-04 Bauer Bros Co Pulping system with impregnation digester having liquor recirculation and cleaning loop
WO1995034712A1 (en) * 1994-06-16 1995-12-21 Kamyr, Inc. Improved chip feeding for a continuous digester
US5674359A (en) * 1995-02-08 1997-10-07 Ahlstrom Machinery Inc. Continuous cooking of cellulosic fibrous material with cold alkali impregnation

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3562096A (en) * 1967-04-21 1971-02-09 Lummus Co Recovery of soap fraction from recycle impregnating cooking liquor in a continuous rapid pulping system
SE468053B (sv) * 1988-12-20 1992-10-26 Kamyr Ab Saett vid kontinuerlig uppslutningskokning av cellulosahaltigt fibermaterial
US5053108A (en) * 1989-06-28 1991-10-01 Kamyr Ab High sulfidity cook for paper pulp using black liquor sulfonization of steamed chips
US5236678A (en) * 1990-08-16 1993-08-17 The Dow Chemical Company Process for absorption of sulfur compounds from fluids using piperidines
FR2670512A1 (fr) * 1990-12-17 1992-06-19 Int Patents Corp Systeme d'alimentation en plantes annuelles ou copeaux de bois pour un reacteur de cuisson continu sous pression destine a la production de pate cellulosique.
SE9401769L (sv) * 1994-05-24 1995-11-25 Nils Mannbro Flisimpregnering vid pappersmassakokning med sulfidiskt alkali
US5660686A (en) * 1994-09-02 1997-08-26 Ahlstrom Machinery Inc. Cooking with spent liquor pretreatment of cellulose material
SE9703365D0 (sv) * 1997-09-18 1997-09-18 Kvaerner Pulping Tech Method in connection with impregnation and digestion of lignocelulosic material
CA2318027C (en) * 1999-09-13 2008-07-08 Andritz-Ahlstrom Inc. Treating pulp with yield or strength-enhancing additive
SE518993E (sv) * 2002-01-24 2013-04-23 Metso Paper Sweden Ab Framställning av cellulosamassa genom kokning med en kokvätska innehållande förindunstad svartlut
FI20040637A (fi) * 2004-05-05 2005-11-06 Metso Paper Inc Menetelmä ja laite kaasun poistamiseksi paloiksi pilkotusta materiaalista

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3258390A (en) * 1962-10-20 1966-06-28 Domtar Ltd Method and apparatus for maintaining a water balance during impregnation and digestion of cellulosic material
US3448002A (en) * 1964-06-20 1969-06-03 Domtar Ltd Pulping process
US3814662A (en) * 1969-09-08 1974-06-04 Bauer Bros Co Pulping system with impregnation digester having liquor recirculation and cleaning loop
US3802956A (en) * 1970-03-17 1974-04-09 Kamyr Ab Method for impregnation of cellulosic fiber material with digesting liquor while preventing dilution of said liquor
WO1995034712A1 (en) * 1994-06-16 1995-12-21 Kamyr, Inc. Improved chip feeding for a continuous digester
US5674359A (en) * 1995-02-08 1997-10-07 Ahlstrom Machinery Inc. Continuous cooking of cellulosic fibrous material with cold alkali impregnation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP1797235A4 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2265759A1 (en) * 2006-11-07 2010-12-29 Metso Fiber Karlstad AB Method for an energy efficient production of cellulose pulp in a continuous digester
EP2265759A4 (en) * 2006-11-07 2013-01-09 Metso Paper Sweden Ab PROCESS FOR PRODUCTION OF CELLULOSE PULP WITH EFFICIENT ENERGY MANAGEMENT IN A CONTINUOUS WASHING MACHINE
AU2008203206B2 (en) * 2007-08-07 2011-12-15 Andritz Inc. Method and System for Semi-Chemical Pulping
WO2011138633A1 (en) * 2010-05-04 2011-11-10 Bahia Specialty Cellulose Sa Method and system for pulp processing using cold caustic extraction with alkaline filtrate reuse
US8535480B2 (en) 2010-05-06 2013-09-17 Bahia Specialty Cellulose Sa Method and system for pulp processing using cold caustic extraction with alkaline filtrate reuse
US8734612B2 (en) 2010-05-06 2014-05-27 Bahia Specialty Cellulose Method and system for high alpha dissolving pulp production
EP3124693A1 (fr) * 2015-07-31 2017-02-01 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif et procede de traitement de la liqueur noire provenant de la preparation de pate a papier par liquefaction hydrothermale
FR3039567A1 (fr) * 2015-07-31 2017-02-03 Commissariat Energie Atomique Dispositif et procede de traitement de la liqueur noire provenant de la preparation de pate a papier par liquefaction hydrothermale
US10407827B2 (en) 2015-07-31 2019-09-10 Commissariat A L'energie Atomique Et Aux Energies Alternatives Device and method for treating the black liquor resulting from pulping by hydrothermal liquefaction
EP3377696A4 (en) * 2015-11-16 2019-08-21 Valmet AB METHOD FOR HEATING CELLULOSE MATERIAL AT FULL COOKING TEMPERATURE IN CELLULOSE COOKERS

Also Published As

Publication number Publication date
CN101068977B (zh) 2011-05-11
FI20041288A0 (fi) 2004-10-04
CA2581923A1 (en) 2006-04-13
EP1797235A1 (en) 2007-06-20
FI20041288A (fi) 2006-04-05
EP1797235A4 (en) 2010-10-06
FI120547B (fi) 2009-11-30
US20070256801A1 (en) 2007-11-08
CN101068977A (zh) 2007-11-07

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