EP2751331A1 - Kraft cooking method using polysulfide cooking liquor - Google Patents
Kraft cooking method using polysulfide cooking liquorInfo
- Publication number
- EP2751331A1 EP2751331A1 EP20110871390 EP11871390A EP2751331A1 EP 2751331 A1 EP2751331 A1 EP 2751331A1 EP 20110871390 EP20110871390 EP 20110871390 EP 11871390 A EP11871390 A EP 11871390A EP 2751331 A1 EP2751331 A1 EP 2751331A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cooking
- liquor
- polysulfide
- impregnation stage
- concentration
- Prior art date
- 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.)
- Granted
Links
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
- D21C1/00—Pretreatment of the finely-divided materials before digesting
- D21C1/06—Pretreatment of the finely-divided materials before digesting with alkaline reacting compounds
-
- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
Definitions
- the present invention relates to a method for the preparation of kraft pulp with increased pulping yield from lignin-containing cellulosic material using polysulfide cooking liquor.
- Cooking methods was therefore developed in order to reduce the detrimental high alkali peak concentrations at start of the cook, and thus was split charges of alkali during the cook implemented in cooking methods such as MCC, EMCC, ITC and Lo-Solids cooking.
- Metso disclosed a pretreatment stage using polysulfide cooking liquor ahead of black liquor treatment.
- the polysulfide treatment liquor drained after the pretreatment stage and before starting the black liquor treatment.
- the polysulfide treatment stage was also preferably kept short with treatment time in the range 2- 10 minutes.
- the invention is based upon the surprising finding that concentration of polysulfide should be kept high in a low temperature pretreatment stage at relatively long retention time before cooking, using liquor to wood ratios well below that as commonly used.
- the stabilization effect of carbohydrates the major objective for polysulfide addition, has shown to be improved dramatically if using a liquor to wood ratio of about 2,9 instead of the conventional liquor to wood ratio of about 3,5, and all other conditions equal. This non proportional effect of low liquor to wood ratio has not been disclosed or realized before despite the numerous proposals for improving cooking yield using polysulfide cooking liquor.
- One object of the present invention is to provide an improved method for the preparation of kraft pulp with increased pulping yield from lignin-containing cellulosic material using polysulfide cooking liquor, wherein the lignin-containing cellulosic material is heated to a temperature in the range 50-100 °C followed by adding polysulfide cooking liquor to a first impregnation stage which in turn is followed by cooking stages resulting in a kraft pulp with a kappa number below 40, and wherein the impregnation stage is conducted at high alkali concentration, low temperature and high polysulfide concentration using polysulfide cooking liquor at a liquor-to-wood ratio in the range 2.0 to 3.2 , and that the temperature is between 80-120 °C during a retention time resulting in a h-factor in the range 2-20 and preferably 2-10 of the impregnation stage.
- This low h-factor is indicative for that no cooking or delignification effect is obtained in the first impregnation stage, and hence is no reduction in pulp viscosity seen as could be the case if high alkali concentrations are at hand in cooking stages at higher temperatures.
- the method is the effective alkali concentration during the impregnation stage above 60 g/l when adding the polysulfide cooking liquor.
- the polysulfide concentration during the impregnation stage above 3 g/l, or above 0,09 mol/l, when adding the polysulfide cooking liquor.
- the method is more than 90% of the total charge of cooking liquor needed for completion of the cooking stages to the intended kappa number below 40 charged to the first impregnation stage, and that at least 175 kg of alkali (EA as NaOH) per ton of chips is charged for softwood and at least 160 kg of alkali per ton of chips for hardwood.
- EA alkali
- the alkali concentration reduced by at least 8 g/l by adding additional cooking liquids having less alkali concentration than the alkali concentration prevailing at end of the first impregnation stage when increasing the temperature to cooking temperature, said cooking liquids in at least part thereof includes black liquor.
- the inventive method has also preferably the white liquor added to the first impregnation stage an alkali concentration above 100 g/l and a polysulfide concentration above 4 g/l.
- the lignin-containing cellulosic materials to be used in the present process are suitably softwood, hardwood, or annual plants.
- FIG. 1 is a schematic cooking system capable of implementing the inventive method
- FIG. 2 demonstrate an example of the alkali profile established with the inventive method ;
- FIG. 3 show the dramatic impact on increased yield when increasing the polysulfide concentration above 0.15 mol/L
- FIG. 4 show the relative stabilization of carbohydrates as a function of liquid to wood ratio during the impregnation stage.
- FIG 1 a 2-vessel kraft cooking system, having a first hydraulic impregnation vessel B and a second steam/liquid phase digester C, wherein the inventive method could be implemented.
- this type of system is first the lignin containing cellulosic material Ch fed to a bin A wherein the cellulosic material is heated to a temperature in the range 50-100 °C by using addition of steam St.
- the lignin containing cellulosic material could preferably be wood chips.
- the treatment liquor here is preferably only polysulfide cooking liquor, WL, and preferably is the entire charge of cooking liquor needed for the cooking process charged here.
- the chips suspended in the treatment liquor are fed to the sluice feeder and displaced liquid is fed out from the bottom outlet of the sluice feeder and returned to the chute in a low pressure circulation.
- the chips in the sluice feeder is pressurized by the return flow from the vessel B and fed out to the top separator TS in top of the vessel B.
- the first impregnation stage is implemented in the vessel B and preferably only with the polysulfide cooking liquor and as small amount as possible of additional liquids such as wood moisture, steam condensates, and especially no black liquor nor additional water or filtrates.
- the resulting liquor-to-wood ratio established should be in the range 2.0 to 3.2 and the temperature should be in the range 80-120 ⁇ .
- the impregnated chips will be fed to the steam/liquid phase digester C together with the residual treatment liquor.
- a conventional transfer system with dilution in bottom of the vessel B using withdrawn treatment liquor from the top separator TS in the top of vessel C.
- the chip suspension heated to full cooking temperature, in the range 140-170 ⁇ depending upon type of cellulosic material, and additional liquid is added in order to reduce the alkali concentration at this point.
- a digester C with 2 concurrent cooking zones, one cooking zone above the first screen section and a second cooking zone above the final screen section in bottom of digester.
- a final counter current wash zone implemented in bottom of digester by addition of wash water/Wash.
- the final pulp with a kappa number below 40 is fed out from bottom in flow Pu.
- figure 2 is disclosed the alkali concentration profile that could be established in a system like that disclosed in figure 1 , with alkali consumption of about 1 10 kg/BDT in the
- impregnation vessel 45 kg/BDT in the first cooking zone in vessel C and 15 kg/BDT in last cooking zone in vessel C.
- an alkali In the top of the first impregnation vessel B is an alkali
- figure 3 is disclosed the improved carbohydrate yield as a function of the polysulfide concentration, when about 1 % lignin is still present in the pulp.
- the dramatic increase in yield when increasing the polysulfide concentration above 0,15 mol/L There is basically a linearly increasing yield when the concentration increases between 0 to 0,15 mol/l. In this initial range is the yield increased from about 45% up to about 46.2%. However, when the concentration reach 0,2 mol/L is the yield increased to about 48,3%.
- a series of tests has been made simulating a system as that shown in figure 1 using a white liquor having an alkali concentration of about 1 17 g/L and a polysulfide concentration of about 6 g/l.
- the charges of flows to the first impregnation stage are in tests #1 -7 using part flows a-e. This results in a liquor to wood ratio shown in row L/W.
- each polysulfide ion can be considered to consist of one atom "sulfide sulfur", i.e. sulfur in the formal oxidation state S(-ll), and n atoms of polysulfide "excess sulfur”, i.e. sulfur in the formal oxidation state S(0).
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
Abstract
Description
Claims
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/SE2011/051038 WO2013032377A1 (en) | 2011-08-30 | 2011-08-30 | Kraft cooking method using polysulfide cooking liquor |
Publications (4)
| Publication Number | Publication Date |
|---|---|
| EP2751331A1 true EP2751331A1 (en) | 2014-07-09 |
| EP2751331A4 EP2751331A4 (en) | 2015-05-20 |
| EP2751331B1 EP2751331B1 (en) | 2017-06-14 |
| EP2751331B2 EP2751331B2 (en) | 2020-04-22 |
Family
ID=47756632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP11871390.8A Active EP2751331B2 (en) | 2011-08-30 | 2011-08-30 | Kraft cooking method using polysulfide cooking liquor |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20140299283A1 (en) |
| EP (1) | EP2751331B2 (en) |
| JP (1) | JP5989777B2 (en) |
| CN (1) | CN103827388B (en) |
| WO (1) | WO2013032377A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2750703T3 (en) * | 2014-08-26 | 2020-03-26 | Valmet Oy | Cost-effective kraft firing procedure using a polysulfide firing liquor |
| FI129362B (en) | 2017-05-16 | 2021-12-31 | Andritz Oy | Method for producing chemical pulp |
| SE1950606A1 (en) * | 2019-05-22 | 2020-10-13 | Valmet Oy | A method for extracting hydrolysate, a batch cooking system and a hydrolysate extracting arrangement |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3567572A (en) | 1967-09-06 | 1971-03-02 | Pulp Paper Res Inst | Polysulfide liquor impregnation of lignocellulose materials in a multistage pulping process |
| NO131612C (en) * | 1969-12-09 | 1975-06-25 | Pulp Paper Res Inst | |
| US3664919A (en) * | 1969-12-09 | 1972-05-23 | Pulp Paper Res Inst | Vapor phase polysulphide liquid pulping of lignocellulosic materials |
| JP3064607B2 (en) * | 1991-11-25 | 2000-07-12 | 王子製紙株式会社 | Modified Kraft Pulp Production Method |
| US5660686A (en) * | 1994-09-02 | 1997-08-26 | Ahlstrom Machinery Inc. | Cooking with spent liquor pretreatment of cellulose material |
| AU9195598A (en) | 1997-09-18 | 1999-04-05 | Kvaerner Pulping Ab | Polysulfide pulping process |
| JP4298059B2 (en) * | 1999-05-28 | 2009-07-15 | 日本製紙株式会社 | Cooking method of lignocellulosic material |
| SE0104247L (en) | 2001-12-14 | 2002-10-22 | Kvaerner Pulping Tech | Pre-treatment of chips with fresh white liquor before treatment with black liquor |
| US7828930B2 (en) * | 2007-11-20 | 2010-11-09 | International Paper Company | Use of polysulfide in modified cooking |
| JP4629164B2 (en) * | 2009-05-26 | 2011-02-09 | 日本製紙株式会社 | Cooking method of lignocellulosic material |
-
2011
- 2011-08-30 WO PCT/SE2011/051038 patent/WO2013032377A1/en not_active Ceased
- 2011-08-30 JP JP2014528324A patent/JP5989777B2/en active Active
- 2011-08-30 CN CN201180073158.6A patent/CN103827388B/en active Active
- 2011-08-30 US US14/241,141 patent/US20140299283A1/en not_active Abandoned
- 2011-08-30 EP EP11871390.8A patent/EP2751331B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| JP2014525519A (en) | 2014-09-29 |
| JP5989777B2 (en) | 2016-09-07 |
| EP2751331B1 (en) | 2017-06-14 |
| CN103827388B (en) | 2016-09-21 |
| EP2751331B2 (en) | 2020-04-22 |
| US20140299283A1 (en) | 2014-10-09 |
| EP2751331A4 (en) | 2015-05-20 |
| CN103827388A (en) | 2014-05-28 |
| WO2013032377A1 (en) | 2013-03-07 |
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