EP0823948B1 - Procede de production de pulpe d'un materiau cellulosique - Google Patents

Procede de production de pulpe d'un materiau cellulosique Download PDF

Info

Publication number
EP0823948B1
EP0823948B1 EP96914167A EP96914167A EP0823948B1 EP 0823948 B1 EP0823948 B1 EP 0823948B1 EP 96914167 A EP96914167 A EP 96914167A EP 96914167 A EP96914167 A EP 96914167A EP 0823948 B1 EP0823948 B1 EP 0823948B1
Authority
EP
European Patent Office
Prior art keywords
process according
pulp
solvent
formic acid
lignin
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.)
Expired - Lifetime
Application number
EP96914167A
Other languages
German (de)
English (en)
Other versions
EP0823948A1 (fr
Inventor
Sven Siegle
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Natural Pulping AG
Original Assignee
Natural Pulping AG
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 Natural Pulping AG filed Critical Natural Pulping AG
Publication of EP0823948A1 publication Critical patent/EP0823948A1/fr
Application granted granted Critical
Publication of EP0823948B1 publication Critical patent/EP0823948B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/006—Pulping cellulose-containing materials with compounds 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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/003—Pulping cellulose-containing materials with organic compounds

Definitions

  • the invention relates to a method for producing a pulp from cellulose-containing Material.
  • Pulp is understood to be a cellulose pulp that is required for the production of cellulose. This pulp is then used to make paper or cardboard, for example.
  • the pulp-producing industry is finding it increasingly difficult to meet the requirements and requirements relating to environmental protection. In addition, it is no longer permitted, for example in Germany after the environmental regulations of 1990, to use traditional pulp production processes such as the sulfate process.
  • sulfur-containing disintegrants in order to extract the lignin that acts as a composite from the cellulose-containing material, only the sulfite process is used in Germany.
  • the so-called Acetosolv process developed which the digestion liquid contains at least 50% by weight of acetic acid and additionally a small amount of hydrochloric acid. After this information the pulp thus obtained with sodium hydroxide solution and optionally also with organic Solvents washed to make the lignin more or less complete to remove.
  • a disadvantage of this process is the relatively high acetic acid consumption and the use of sodium hydroxide solution and optionally organic solvents for washing the pulp.
  • the pulp obtained in this way is regularly bleached in a subsequent step in order to achieve kappa numbers of at least below 25.
  • downstream bleaching by means of a peroxide is provided, with a relatively high consumption of this bleaching agent being disadvantageous.
  • EP-A-0 325 891 has therefore disclosed an improvement in this acetosolve process.
  • the improvement essentially consists in that the pulp is no longer washed with sodium hydroxide solution after digestion, but with a C 1-3 carboxylic acid or a mixture of such acids and that the subsequent bleaching is also carried out in the acidic medium with additional Use of hydrogen peroxide or ozone is carried out.
  • a carboxylic acid ester such as butyl acetate can also be used as the solvent.
  • the C 1-3 carboxylic acid used for washing the pulp can subsequently be used again as a digestion liquid.
  • WO-A-82/01902 also discloses a process for producing a pulp from cellulose-containing material using formic acid.
  • GB-A-850 367 teaches the use of formic acid in the production of cellulose.
  • WO-A-86/05529 has disclosed a process for producing bleached pulp from cellulose-containing material, which is generally also referred to as the Milox process.
  • the digestion is carried out in a peroxyformyl, peroxyacetic, peroxypropion or peroxybutyric acid medium, the peroxyacid being obtained by mixing the respective acid with a relatively high proportion of hydrogen peroxide and then carrying out the digestion process.
  • This digestion is followed by bleaching of the pulp, which is carried out in an alkaline solution to which hydrogen peroxide has been added.
  • the disadvantage of this process is again the use of an alkaline solution such as sodium hydroxide solution and the high proportion of hydrogen peroxide required.
  • the present invention has for its object to provide a method for producing a pulp from cellulose-containing material that works as environmentally friendly as possible and at the same time extremely economical and efficient.
  • the method according to the invention as claimed in claim 1 is used, for example, when the cellulose-containing material used is not so easy to digest. This is the case, for example, with hardwood or coniferous wood, but also with grain straw, depending on the intended use of the pulp obtained from it.
  • the cellulosic material is mixed with formic acid and water and heated slightly under reflux by an external energy source. Then hydrogen peroxide is slowly added in a constant dosage.
  • Such a procedure has hitherto not been known by any prior art and enables a very economical procedure because the now exothermic reaction itself provides the heat necessary for cooking.
  • Digestion solution is understood to mean the sum of the solvent, the cellulose-containing material and components, such as lignin and sugar, that may have been extracted therefrom. Furthermore, in the reaction according to the preferred embodiment it is advantageous that the equilibrium in the reaction of the formation of the peracid from formic acid and hydrogen peroxide is continuously shifted to the peracid side by the continuous addition of the hydrogen peroxide.
  • aqueous formic acid can be combined in one Concentration range between about 60 to 99% by weight can be used.
  • the use of 100% formic acid is not cheap, because at least one certain percentage of water in the manufacture of the pulp, i.e. in the digestion process should be present.
  • the cooking time can be a period of can be given in about 30 to 120 minutes, depending on the cellulose-containing used Material.
  • the predetermined amount of hydrogen peroxide can be about 1 to 3 % By weight, preferably 1 to 2% by weight, particularly preferably 1% by weight on the total weight of cellulosic material and solvent be. It is particularly advantageous here that only a very small amount of added hydrogen peroxide is necessary, which is sufficient to the one hand Requirements for the whiteness of the pulp so produced for the production of paper and which, on the other hand, is sufficient to withstand the temperature of the To keep the digestion solution approximately at the boiling point of the solvent, without supplying additional energy in the form of heat. So that can good properties of the paper made from the pulp can be combined with a minimal expenditure of energy.
  • the method according to the invention can further be modified in this regard be that in addition to the solvent a gas such as air, oxygen, ozone or a comparable gas or a mixture of two or more of these Gases is introduced.
  • a gas such as air, oxygen, ozone or a comparable gas or a mixture of two or more of these Gases is introduced.
  • the oxidative power of these gases is used, which increases lignin degradation and thus whiteness, as well as the kappa number lowers.
  • the required digestion time is also reduced.
  • the pulp can be easily removed after the cooking time Sieves are separated from the solvent.
  • This will sieve understood in the broadest sense, i.e. a separation by a suitable one Membrane, a filter or a frit is also possible, but then that Disconnection can happen continuously.
  • the pulp so screened can then be washed with water and / or formic acid. Especially when Washing with formic acid becomes the remaining lignin, which is already out the cellulose-containing material is dissolved out. By opening the pulp by means of a stirrer can still flush this out be promoted.
  • the cooking temperature is reduced.
  • Aqueous formic acid is then used as the solvent, to which hydrogen peroxide, as already described above, is added.
  • the reduced cooking temperature can be around 70 to 80 ° C.
  • the cooking temperature is preferably 70 ° C., since at this temperature there is an optimum of performic acid.
  • the cooking time can be extended to up to 5 hours to achieve a higher degree of whiteness.
  • the cooking time is then preferably about 3 hours, because it was found that after this time the pulp no longer brightened up appreciably. It has also proven advantageous to increase the liquid-to-material ratio to over 25: 1.
  • elephant grass can be used as a cellulose-containing material. and / or corn leaves or stems are used. Both materials, in particular Elephant grass can be easily unlocked. It can even the addition of hydrogen peroxide to the solvent can be dispensed with. For example, when using 99% formic acid and one Cooking time of one hour reaches a kappa number of 4.7.
  • a particular advantage of the method according to the invention is, however, that as cellulosic material basically annual plants, especially cereal straw, can be used. This is especially true for papermaking important, because so far almost exclusively as a cellulosic material Wood is used. Worldwide there are over 200 million a year Tons of paper used. The demand continues to grow. The deforestation large forest areas to cover the need for cellulose-containing material but brings significant environmental problems such as climate change and habitat destruction of flora and fauna with them. Where, if any, Reforestation is usually only rapidly growing Monocultures created, which in turn are very pest-prone and ecological are not useful. In addition, developing countries or countries of the so-called "third world" an increasing need for paper for the determine various purposes.
  • the process according to the invention is also based on the cellulose-containing processes which have been customary to date Materials such as hardwood or softwood can be used. You know that it is generally more difficult with these materials, an adequate one To provide the whiteness of the paper made from the pulp, it then lends itself, according to the particularly preferred embodiment to proceed and the inventive method while reducing the Repeat cooking temperature and optional extension of cooking time.
  • Another aspect of the present invention relates to that from pulp the process of the invention lignin. This is after the Recycling of formic acid used as a solvent by simple Distillation obtained from the distillation residue by precipitation in water. This precipitation of the water-insoluble lignin at the same time makes it of the water-soluble sugars also present in the residue separated.
  • the pulp thus obtained is used for pulp production for example for the paper industry or for the production of Cardboard used.
  • manufactured pulp can be used and used wherever pulp is used Starting material for a product is required. For example Chemical cellulose or any other product from regenerated or chemical modified cellulose from the pulp.
  • Lignin which by the inventive method is available can be safely processed as it is contains no sulfur or chlorine, as is the case in the prior art known methods for producing a pulp would mostly be the case.
  • the Isolated lignin can be used, for example, as a construction material, in particular as Starting material for pressboard, medium density fibreboard or as filler be used if it decomposes with excess oxalic acid and either melted or boiled in a saturated formic acid solution and then steamed with cellulose fiber. This creates a waterproof black-brown mass.
  • lignin is even more diverse. So it can be used as a raw material for the production of flavorings such as vanillin or mulled wine flavor.
  • Cereal straw, formic acid and water are transferred into the reaction vessel in accordance with the percentages by weight given below and in accordance with the liquid-to-straw ratio also given there.
  • this is a round bottom flask, combined with a ground thermometer and a dimrotre reflux condenser.
  • the reaction mixture is then heated slightly under reflux and then hydrogen peroxide of the concentration given below is slowly added continuously.
  • the reaction is exothermic, so that the external energy supply, such as here via a heating pad or a heating plate, can at least initially be reduced and then completely eliminated.
  • the digestion time is also given below.
  • the pulp is separated from the pulping solution by simple sieving and mixed with further fresh formic acid in a concentration of 60 to 80% by weight, so as to flush out the remaining lignin.
  • a paddle stirrer is then inserted into the reaction vessel and stirred for about one minute. This creates a defibrillation of the cellulose dressings and the lignin washout is facilitated.
  • the formic acid is recovered with the formic acid from the digestion by simple distillation. Again on a laboratory scale, a Liebig distillation apparatus and a 300 mm column were used. The formic acid used can largely be recovered here. Usually in a percentage of over 95%.
  • test parameters shown indicate optimized production processes, although the optimization in test 3.a) was carried out in such a way that not only was a maximum lignin removal achieved, but the lignin itself should also be obtained in as large a quantity as possible. It has been shown that optimal lignin removal is accompanied by an increased breakdown of the lignin to water solubility. The optimization was therefore carried out in such a way that lignin which had not been broken down or altered as far as possible should be obtained in addition to the lignin-free pulp.
  • the described manufacturing possibilities of a pulp can still be achieved be improved that a gas is used in addition to the digestion like air, oxygen, ozone or the like, for its oxidative power to exploit in the digestion. Also a mixture of two or more the gases mentioned can be used.
  • the digestion process described above or one of its variants is then carried out so that additionally into the reaction vessel from below the appropriate gas type or a gas mixture using a wide nozzle is initiated. This can be done continuously or discontinuously.
  • the escaping gas can then be used again or disposed of in an environmentally friendly manner using the known methods become.
  • an excess of oxalic acid is added to the lignin and melted or according to another process variant in saturated formic acid solution cooked and then evaporated with cellulose fibers.
  • a waterproof black-brown mass that can be used as a filler or after Type of pressboard or fiberboard can be used.

Landscapes

  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Claims (18)

  1. Procédé de fabrication d'une pâte de bois en matériau contenant de la cellulose, lors duquel le matériau est mélangé à de l'acide formique en tant que solvant et est légèrement chauffé sous reflux par une source d'énergie externe et est alors lentement et, pour l'essentiel, sans apport d'énergie externe supplémentaire, mélangé à du peroxyde d'hydrogène sous un dosage constant, de telle sorte que le matériau soit cuit sous reflux à environ la température d'ébullition du solvant.
  2. Procédé selon la revendication 1, lors duquel l'on utilise, en tant que solvant, de l'acide formique aqueux dans un domaine de concentration compris entre environ 60 et 99% en poids.
  3. Procédé selon l'une quelconque des revendications 1 ou 2, lors duquel la durée de cuisson est environ de 120 minutes.
  4. Procédé selon l'une quelconque des revendications 2 ou 3, lors duquel la quantité prédéterminée de peroxyde d'hydrogène est environ de 1 - 3% en poids, de préférence de 1 - 2% en poids, en particulier de préférence de 1% en poids, par rapport au poids total du matériau contenant de la cellulose et du solvant.
  5. Procédé selon l'une quelconque des revendications 1 à 4, lors duquel le rapport liquide à matériau est compris entre environ 20:1 et 25:1.
  6. Procédé selon l'une quelconque des revendications 1 à 5, lors duquel l'on introduit, dans le solvant, en sus, de l'air, de l'oxygène ou de l'ozone.
  7. Procédé selon l'une quelconque des revendications 1 à 6, lors duquel la pâte de bois est séparée du solvant après achèvement de la durée de cuisson.
  8. Procédé selon la revendication 7, lors duquel la séparation de la pâte de bois se fait par tamisage.
  9. Procédé selon l'une quelconque des revendications 8 ou 9, lors duquel la pâte obtenue est lavée à l'aide d'eau et/ou d'acide formique.
  10. Procédé selon l'une quelconque des revendications 7 à 9, lors duquel l'acide formique est récupéré par recyclage au moins partiellement, de préférence jusqu'à au-delà de 95% en poids, le recyclage se faisant par distillation simple.
  11. Procédé selon l'une quelconque des revendications 1 à 9, qui est répété, la température de cuisson étant diminuée.
  12. Procédé selon la revendication 11, lors duquel la température de cuisson diminuée est environ de 70 - 80°C, de préférence de 70°C.
  13. Procédé selon la revendication 11 ou 12, lors duquel la durée de cuisson est prolongée et est environ de 1-5 heures, de préférence de 3 heures.
  14. Procédé selon l'une quelconque des revendications 11 à 13, lors duquel le rapport liquide à matériau est augmenté à une valeur au-delà de 25:1.
  15. Procédé selon la revendication 1, lors duquel l'on utilise, en tant que matériau contenant de la cellulose, de l'herbe à éléphant et/ou des feuilles ou des tiges de mais.
  16. Procédé selon l'une quelconque des revendications 1 à 14, lors duquel l'on utilise, en tant que matériau contenant de la cellulose, des plantes annuelles, en particulier de la paille de blé.
  17. Procédé selon l'une quelconque des revendications 1 à 14, lors duquel l'on utilise, en tant que matériau contenant de la cellulose, du bois de feuillus ou de sapins.
  18. Procédé selon la revendication 10, lors duquel le résidu de distillation contient de la lignine, qui est isolée par précipitation dans l'eau.
EP96914167A 1995-05-03 1996-05-02 Procede de production de pulpe d'un materiau cellulosique Expired - Lifetime EP0823948B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19516151A DE19516151A1 (de) 1995-05-03 1995-05-03 Verfahren zur Herstellung einer Pulpe aus zellulosehaltigem Material, die Pulpe selbst und deren Verwendung
DE19516151 1995-05-03
PCT/EP1996/001823 WO1996035013A1 (fr) 1995-05-03 1996-05-02 Procede de production de pulpe d'un materiau cellulosique, pulpe obtenue et son utilisation

Publications (2)

Publication Number Publication Date
EP0823948A1 EP0823948A1 (fr) 1998-02-18
EP0823948B1 true EP0823948B1 (fr) 2002-04-03

Family

ID=7760931

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96914167A Expired - Lifetime EP0823948B1 (fr) 1995-05-03 1996-05-02 Procede de production de pulpe d'un materiau cellulosique

Country Status (12)

Country Link
US (1) US6183597B1 (fr)
EP (1) EP0823948B1 (fr)
JP (1) JP3059998B2 (fr)
CN (1) CN1098390C (fr)
AT (1) ATE215632T1 (fr)
CA (1) CA2217987A1 (fr)
DE (2) DE19516151A1 (fr)
DK (1) DK0823948T3 (fr)
ES (1) ES2175091T3 (fr)
PT (1) PT823948E (fr)
RU (1) RU2139965C1 (fr)
WO (1) WO1996035013A1 (fr)

Families Citing this family (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI103588B (fi) * 1996-01-19 1999-07-30 Esa Rousu Consulting Oy Menetelmä tekokuitujen ja muiden kuitujen raaka-aineen valmistamiseksi ruohovartisista kasveista
FR2770543B1 (fr) * 1997-10-30 2000-05-05 Michel Delmas Procede de production de pate a papier, lignignes sucres et acide acetique par fractionnement de matiere vegetale lignocellulosique em milieu acide formique/acide acetique
RU2145986C1 (ru) * 1998-08-25 2000-02-27 Иоссель Юрий Яковлевич Способ изготовления целлюлозы
US7402224B1 (en) 1999-05-06 2008-07-22 Compagnie Industrielle De La Matiere Vegetale Method for producing paper pulp, lignins, sugars and acetic acid by frantionation of lignocellulosic vegetable material in formic/acetic acid medium
DE10057878A1 (de) * 2000-11-21 2003-02-27 Natural Pulping Ag I Ins Verfahren zur Herstellung einer Pulpe aus cellulosehaltigem Material
DE19962411A1 (de) * 1999-12-22 2001-07-05 Natural Pulping Ag Verfahren zur Gewinnung/Rückgewinnung von Carbonsäuren aus Ablaugen der Zellstoffherstellung
FI108234B (fi) * 2000-02-28 2001-12-14 Chempolis Oy Menetelmä massan valmistamiseksi
EP1299595A4 (fr) * 2000-06-29 2004-06-23 Bncompulp Co Ltd Procede de preparation de la pate a papier a partir de tiges de mais
DE10057910C2 (de) * 2000-11-21 2003-02-06 Advanced Recovery Technologies Verfahren zur Derivatisierung von technischem Lignin, derivatisiertes technisches Lignin und dessen Verwendung
US20080185293A1 (en) * 2002-03-27 2008-08-07 Giselher Klose Method and Apparatus for Decontamination of Fluid with One or More High Purity Electrodes
US7691253B2 (en) * 2002-03-27 2010-04-06 Ars Usa Llc Method and apparatus for decontamination of fluid
US7695607B2 (en) * 2002-03-27 2010-04-13 Ars Usa Llc Method and apparatus for decontamination of fluid
CN100485393C (zh) * 2004-09-09 2009-05-06 华南理工大学 一种无污染的高纯度纤维素的分离分析方法
US7270794B2 (en) * 2005-03-30 2007-09-18 Shipley Larry W Process for recovering useful products and energy from siliceous plant matter
KR101292611B1 (ko) * 2005-04-20 2013-08-05 다우 코닝 코포레이션 종이 생산에 사용된 재생 섬유들로부터 유기 침착물의 제거방법
FR2885371B1 (fr) * 2005-05-03 2007-08-03 Cie Ind De La Matiere Vegetale Installation pour la mise en oeuvre d'un procede de production de pate a papier, de lignines et de sucres et procede de production au moyen d'une telle installation
FI123165B (fi) * 2007-11-16 2012-11-30 Jvs Polymers Oy Menetelmä ja laitteisto jatkuvatoimiseksi biomassan molekyylien pilkkomiseksi
WO2009080737A2 (fr) * 2007-12-21 2009-07-02 Shell Internationale Research Maatschappij B.V. Procédé pour convertir de la lignocellulose en sucres
FR2926824A1 (fr) * 2008-01-25 2009-07-31 Cie Ind De La Matiere Vegetale Procede de pretraitement d'une matiere vegetale lignocellulosique en vue de la production de bioethanol.
US20090312537A1 (en) * 2008-04-30 2009-12-17 Xyleco, Inc. Carbohydrates
RU2535222C2 (ru) * 2008-09-08 2014-12-10 Басф Се Способ интегрированного получения целлюлозы и пригодных для повторного использования низкомолекулярных веществ
WO2012125057A1 (fr) * 2011-03-17 2012-09-20 Maksimov Vladimir Vladimirovich Procédé de traitement de matériau fibreux
EP2694723A1 (fr) 2011-04-01 2014-02-12 University of Limerick Traitement de la lignocellulose
FI123052B (fi) * 2011-09-23 2012-10-15 Chempolis Oy Esikäsittelymenetelmä vesiliukoisten sokereiden tuottamiseksi lignoselluloosamateriaalista
CN103898783B (zh) * 2012-12-25 2016-02-10 济南圣泉集团股份有限公司 一种由生物质原料制备纸浆的工艺
CN103898784B (zh) * 2012-12-25 2016-02-10 济南圣泉集团股份有限公司 一种生物质原料的综合利用工艺
EP3148956A4 (fr) * 2014-05-30 2018-01-17 Sulvaris Inc. Engrais à libération lente, à base de biomasse éclatée
BR112018074599A2 (pt) * 2016-06-03 2019-03-19 Kri, Inc. método para produzir fibra fina de celulose
EP3527531A1 (fr) * 2018-02-16 2019-08-21 Michel Delmas Procédé à base de biomasse lignocellulosique pour production de lignines et de gaz de synthèse et gaz de synthèse efficace de production d'électricité
US11618684B2 (en) 2018-09-05 2023-04-04 Kilt, Llc Method for controlling the properties of biogenic silica
CN111393670B (zh) * 2020-03-26 2022-04-05 齐鲁工业大学 一种高效提取分离活性木素的方法

Family Cites Families (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1014536A (fr) * 1940-04-01 1952-08-18 Du Pont Perfectionnements au blanchiment des pâtes de bois
GB555985A (en) * 1942-03-11 1943-09-15 Henry Dreyfus Improvements in or relating to the manufacture of cellulose
BE541737A (fr) 1955-10-01
US3553076A (en) * 1968-01-22 1971-01-05 Weyerhaeuser Co Non-catalytic process for the production of cellulose from lignocellulosic materials using acetic acid
US3654070A (en) * 1970-04-02 1972-04-04 Sterling Drug Inc Oxidation and reuse of effluent from oxygen pulping of raw cellulose
DE2506919C3 (de) * 1975-02-19 1978-10-12 Instituut Voor Bewaring En Verwerking Van Landbouwprodukten, Wageningen (Niederlande) Verfahren zur Gewinnung von ligninreichem Fasermaterial und Verwendung dieses Materials zur Herstellung von Papier und Pappe
SU761647A1 (ru) * 1978-01-30 1980-09-07 Bruss Ti Kirova Способ получения целлюлозного полуфабриката 1
SU821614A1 (ru) * 1979-06-19 1981-04-15 Белорусский Технологический Институт Им.C.M.Кирова Способ получени целлюлозного полу-фАбРиКАТА
DE3005947B1 (de) * 1980-02-16 1981-01-29 Degussa Verfahren zur Bleiche von Zellstoffen mittels organischer Persaeure
JPS597439B2 (ja) 1980-07-31 1984-02-18 株式会社日立製作所 セルロ−ス性物質の前処理方法
WO1982001902A1 (fr) 1980-12-05 1982-06-10 Robert K Jordan Pulpage a l'acide formique
FI74750C (fi) * 1985-03-22 1988-03-10 Keskuslaboratorio Foerfarande foer framstaellning av blekt cellulosamassa utav ligninhaltigt raomaterial.
US4793898A (en) * 1985-02-22 1988-12-27 Oy Keskuslaboratorio - Centrallaboratorium Ab Process for bleaching organic peroxyacid cooked material with an alkaline solution of hydrogen peroxide
FR2593527B1 (fr) * 1986-01-30 1988-03-25 Centre Tech Ind Papier Procede de blanchiment des pates mecaniques.
SE8700569D0 (sv) * 1987-02-12 1987-02-12 Josef Kubat An improved peroxide bleaching method
GB8721528D0 (en) 1987-09-14 1987-10-21 Shell Int Research Pulping lignocellulose-containing material
EP0325891A1 (fr) * 1988-01-25 1989-08-02 Kunz Holding Gmbh & Co. Kg Procédé pour obtenir une pâte de cellulose blanchie
FI80191C (fi) * 1988-03-30 1990-05-10 Valio Meijerien Foerfarande och konserveringsmedel foer ensilering av foder.
FI85510C (fi) 1990-05-29 1992-04-27 Kemira Oy Foerfarande foer aotervinning av laegre alifatisk syra.
FI85511C (fi) 1990-05-29 1992-04-27 Kemira Oy Foerfarande foer aotervinning av alifatiska syror och sockrar.
DE4107354C1 (fr) 1991-03-08 1992-11-05 Acetocell Gmbh & Co Kg, 7162 Gschwend, De
SE470065C (sv) * 1991-04-30 1995-10-12 Eka Nobel Ab Behandling av kemisk massa med en syra och därefter en magnesium- och kalciumförening vid klorfri blekning
ATE168149T1 (de) * 1991-10-04 1998-07-15 Solvay Interox Inc Verfahren zur verbesserung der selektivität bei der delignifizierung von chemischem zellstoff
BE1006057A3 (fr) * 1992-07-06 1994-05-03 Solvay Interox Procede pour la delignification d'une pate a papier chimique.
DE4228171C2 (de) 1992-08-25 1995-06-14 Kaemmerer Projekt Agentur Gmbh Verfahren zur Gewinnung von Zellstoffen

Also Published As

Publication number Publication date
RU2139965C1 (ru) 1999-10-20
ATE215632T1 (de) 2002-04-15
DK0823948T3 (da) 2002-07-29
JPH10511147A (ja) 1998-10-27
WO1996035013A1 (fr) 1996-11-07
ES2175091T3 (es) 2002-11-16
CN1183126A (zh) 1998-05-27
DE19516151A1 (de) 1996-11-07
PT823948E (pt) 2002-08-30
JP3059998B2 (ja) 2000-07-04
EP0823948A1 (fr) 1998-02-18
CN1098390C (zh) 2003-01-08
US6183597B1 (en) 2001-02-06
DE59609018D1 (de) 2002-05-08
CA2217987A1 (fr) 1996-11-07

Similar Documents

Publication Publication Date Title
EP0823948B1 (fr) Procede de production de pulpe d'un materiau cellulosique
DE19916347C1 (de) Verfahren zum Auftrennen lignocellulosehaltiger Biomasse
DE69839097T2 (de) Bleichen von zellstoff mittels persäure
DE69730233T2 (de) Verfahren zur zellstoffherstellung durch einstufiges kochen mit ameisensaüre und wäsche mit perameisensaüre
EP0584675B1 (fr) Délignification de bois à l'acide acétique avec addition d'acide formique
DE102009017051A1 (de) Verfahren zur Gewinnung von Zellstoff aus Lignocellulose-haltiger Biomasse
DE2027319A1 (fr)
DE102006027006A1 (de) Verfahren zum Herstellen von Faserstoff aus Holz
DE2246647A1 (de) Verfahren zur fraktionierten gewinnung von lignin und cellulose aus baumrinde bzw. borke
DE19856582C1 (de) Verfahren zur Gewinnung von Chemiezellstoff aus Hackschnitzeln
EP2029806A2 (fr) Procédé de préparation de matière fibreuse
DE4129739A1 (de) Chlorfreies bleichen von papierpulpe
DE3445132C2 (fr)
EP0325891A1 (fr) Procédé pour obtenir une pâte de cellulose blanchie
DE2128723A1 (de) Verfahren zum Bleichen von Holz pulpe
DE2754991A1 (de) Verfahren zur herstellung von zellstoff
WO2009015699A1 (fr) Matière fibreuse lignocellulosique issue de plantes annuelles
DE2506919C3 (de) Verfahren zur Gewinnung von ligninreichem Fasermaterial und Verwendung dieses Materials zur Herstellung von Papier und Pappe
DE102006061480A1 (de) Verfahren zum Herstellen von Faserstoff
AT404478B (de) Celluloseherstellung
AT398990B (de) Verfahren zur hydrolyse von pflanzenmaterialien
DE102019001184B4 (de) Verfahren zur Herstellung von Papier auf Basis von mittels eines schonenden Extraktionsverfahrens aus aquatischen Makrophyten, insbesondere Wasserpest (Elodea), isolierter Cellulose und durch dieses Verfahren hergestelltes Papier
DE3423024A1 (de) Holzaufschluss mit essigsaeure und chlorethanol
DE3526695A1 (de) Verfahren zur ligninentfernung bei faserstoffen
DE524298C (de) Verfahren zur Herstellung hochwertiger Faserhalbstoffe

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19971103

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI NL PT SE

AX Request for extension of the european patent

Free format text: AL PAYMENT 971103;LT PAYMENT 971103;LV PAYMENT 971103;SI PAYMENT 971103

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: NATURAL PULPING GMBH & CO. KG

RIN1 Information on inventor provided before grant (corrected)

Inventor name: SIEGLE, SVEN

17Q First examination report despatched

Effective date: 19990727

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: NATURAL PULPING AG

RIC1 Information provided on ipc code assigned before grant

Free format text: 7D 21C 3/04 A

RTI1 Title (correction)

Free format text: METHOD OF PRODUCING A PULP OF CELLULOSIC MATERIAL

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

111Z Information provided on other rights and legal means of execution

Free format text: 20011127 AT BE CH DE DK ES FI FR GB GR IE IT LI NL PT SE

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI NL PT SE

AX Request for extension of the european patent

Free format text: AL PAYMENT 19971103;LT PAYMENT 19971103;LV PAYMENT 19971103;SI PAYMENT 19971103

REF Corresponds to:

Ref document number: 215632

Country of ref document: AT

Date of ref document: 20020415

Kind code of ref document: T

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REF Corresponds to:

Ref document number: 59609018

Country of ref document: DE

Date of ref document: 20020508

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: GERMAN

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20020528

REG Reference to a national code

Ref country code: DK

Ref legal event code: T3

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: E. BLUM & CO. PATENTANWAELTE

ET Fr: translation filed
REG Reference to a national code

Ref country code: PT

Ref legal event code: SC4A

Free format text: AVAILABILITY OF NATIONAL TRANSLATION

Effective date: 20020531

REG Reference to a national code

Ref country code: GR

Ref legal event code: EP

Ref document number: 20020402307

Country of ref document: GR

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2175091

Country of ref document: ES

Kind code of ref document: T3

REG Reference to a national code

Ref country code: GB

Ref legal event code: 732E

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20030106

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IE

Payment date: 20030417

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GR

Payment date: 20030422

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20030430

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20030507

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: PT

Payment date: 20030513

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20030514

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FI

Payment date: 20030515

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20030516

Year of fee payment: 8

Ref country code: CH

Payment date: 20030516

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DK

Payment date: 20030520

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20030523

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20030529

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20030530

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 20030715

Year of fee payment: 8

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040502

Ref country code: FI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040502

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040502

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040503

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040503

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040503

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040531

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040531

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040531

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040601

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20041102

BERE Be: lapsed

Owner name: *NATURAL PULPING A.G.

Effective date: 20040531

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20041201

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20041203

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20040502

EUG Se: european patent has lapsed
REG Reference to a national code

Ref country code: DK

Ref legal event code: EBP

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20050131

REG Reference to a national code

Ref country code: PT

Ref legal event code: MM4A

Effective date: 20041102

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 20041201

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.

Effective date: 20050502

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20040503

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20051126

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040531