EP0672207B1 - Verfahren zur herstellung von viskosezellstoffen - Google Patents

Verfahren zur herstellung von viskosezellstoffen Download PDF

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Publication number
EP0672207B1
EP0672207B1 EP94900624A EP94900624A EP0672207B1 EP 0672207 B1 EP0672207 B1 EP 0672207B1 EP 94900624 A EP94900624 A EP 94900624A EP 94900624 A EP94900624 A EP 94900624A EP 0672207 B1 EP0672207 B1 EP 0672207B1
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EP
European Patent Office
Prior art keywords
hsl
digestion
temperature
process according
digester
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
EP94900624A
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German (de)
English (en)
French (fr)
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EP0672207A1 (de
Inventor
Wolfgang Wizani
Andreas Krotscheck
Johann Schuster
Karl Lackner
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.)
Lenzing AG
Primetals Technologies Austria GmbH
Original Assignee
Lenzing AG
Voest Alpine Industrienlagenbau GmbH
Chemiefaser Lenzing AG
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    • 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
    • D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing 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
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam

Definitions

  • the present invention relates to a process for the production of viscose pulp by a steam pre-hydrolysis sulfate (power) displacement cooking process.
  • Viscose pulps are pulps that are used to manufacture rayon, cellophane, carboxymethyl cellulose, nitrocellulose, cellulose acetate, textile fibers and special papers.
  • the special characteristics of the viscose pulp are the high purity and the high content of alpha cellulose.
  • Viscose pulps have a high content of alpha cellulose, a low content of hemicellulose, lignin, ash and extraction substances. The removal of the hemicellulose in the digestion process is particularly difficult since the pentosans are almost as resistant to alkali and acids as the cellulose itself.
  • the alpha cellulose content is determined by dissolving the cellulose in 18% NaOH.
  • Alpha cellulose is the part of cellulose that is not soluble in 18% NaOH.
  • Beta cellulose is the part of the cellulose that precipitates when the 18% solution is subsequently diluted and acidified.
  • Gamma cellulose refers to the part of the substances dissolved in the 18% NaOH that does not fail when the solution is neutralized.
  • a rough guideline can be that alpha cellulose is the cellulose normally present in the plant, while beta cellulose is a measure of the cellulose broken down during chemical digestion and gamma cellulose is a measure of the remaining hemicellulose content.
  • the requirements for the alpha cellulose content differ.
  • rayon for example, an alpha cellulose content of 88-91 is sufficient.
  • viscose pulps that are to be used for cellulose acetate, nitrocellulose or other derivatives must have a much higher alpha content, at least an alpha content of 94-98 and less than 1.5% hemicellulose.
  • Nitrocellulose for explosives are usually made from cotton linters, as this requires an alpha content of over 98% and a hemicellulose content of almost 0%.
  • the hemicelluloses In contrast to paper pulps, where a high hemicellulose content is desirable for reasons of strength, the hemicelluloses must be removed from viscose pulps.
  • the xylans react with CS 2 in the xantonation reaction, and just as quickly as the cellulose itself, which leads to an increased consumption of CS 2 .
  • Other hemicelluloses react more slowly than cellulose and then cause difficulties in filtration.
  • Viscose pulp is mainly produced worldwide using the sulfite process.
  • the acid sulphite process is particularly suitable because of its rapid hydrolysis of hemicellulose and the fairly good delignification rate.
  • bisulfite and neutral sulfite processes are also used in two- or multi-stage processes.
  • the following can be said about the sulfite digestion processes: They are generally carried out as batch cooking, that is to say batchwise.
  • the cooking temperature is in the range of 135 ° C for acid sulfite processes and 160 ° C for bisulfite processes.
  • the pressure of the SO 2 gas in the cooker increases, excess SO 2 is blown off at a given point in time.
  • the digestion takes a total of about 6-8 hours.
  • the essential parameters for determining the end product quality and the yield are the sulfidity, the pH and the temperature.
  • the type of base also has an influence, in particular on the rate of diffusion of the digestion chemicals into the wood chips.
  • the degradation of the hemicelluloses, in particular the xylans and mannans, took place primarily by acid hydrolysis of glucosidic bonds.
  • the degraded hemicelluloses are removed from the pulp with the digestion solution.
  • the degraded celluloses (beta-celluloses) must be removed by a subsequent alkaline treatment.
  • the cellulose in viscose pulps generally has a lower DP than that of paper pulp. This is due to the acidity required for hemicellulose removal, which also partially degrades the cellulose hydrolytically.
  • This lower DP means that sulfite viscose pulps are used for applications with high strength requirements such as e.g. "high tenacity rayon cord" cannot be used.
  • Single-stage sulfite processes are unable to process certain softwoods such as To unlock Douglas fir, larch and most types of pine because of their high resin content.
  • the resin content is particularly present in the heartwood area, so the digestion of sawn wood waste with this process - since it is mostly sapwood - can be considered in some cases.
  • two-stage or multi-stage procedures are used in practice.
  • the first stage is usually less acidic than the second.
  • the lignin is sulfonated in the first stage, which prevents recondensation of the lignin in the second stage, in which primarily the hemicelluloses are removed.
  • the sulfite digestion takes place with various bases, namely calcium, sodium, ammonium and magnesium.
  • the calcium sulfite process is on the verge of extinction because chemical recovery is difficult. Magnesium sulfite processes are common for the production of viscose pulp because of the simple chemical recovery. In multi-stage magnesium sulfite digestion processes, an acidic pH is used in the first stage. Otherwise the digestion conditions in the magnesium sulfite process are largely identical to those of the known calcium sulfite digestion.
  • the first stage is a bisulphite stage with pH 3-4 for the impregnation of the wood chips.
  • the second stage largely corresponds to conventional sulfite digestion, in which SO 2 is added and the viscosity of the pulp is determined. At the end of the second stage, SO 2 is exhausted.
  • sodium carbonate is added to neutralize the cooking liquor. Depending on the temperature and pH conditions, viscose pulps with alpha cellulose contents of 89-95% are produced.
  • the Domsjo process which has been in operation since 1960, is a two-stage process with which high yields of viscose pulp are achieved.
  • the first stage works with a pH of 4.5 - 6, the second stage corresponds to normal acid sulfite digestion.
  • the pH of the second stage is adjusted by adding SO 2 water.
  • yields are achieved which are 2% above that of a one-stage process with correspondingly low sorting losses.
  • the yield can be increased by 4-5%, to 29-35%, but at the expense of a higher glucomannan content.
  • the alpha cellulose content is below the previously described process; it is 83-89% in the one-step process and 85-90% in the two-step process.
  • Higher alpha cellulose contents with a corresponding reduction in the yield can be obtained by post-treatment of the substance with dilute alkali at elevated temperature or with concentrated alkali at room temperature followed by acid treatment in order to remove the remaining inorganic substances.
  • the sulfate (power) digestion process in its usual one-step version is not suitable for the production of viscose pulp. Only 84-86% alpha cellulose are with this Embodiment achievable. Even longer cooking times or higher cooking temperatures do not lead to the goal. These only result in an increased degradation of the cellulose due to alkaline hydrolysis of the glucosidic bonds in connection with the so-called "peeling off reaction”. Combined with an acid pretreatment - the so-called pre-hydrolysis - this alkaline pulping process can be used to produce high-quality viscose pulps from all the raw materials that are common for pulp production. A number of viscose pulp mills use this method, whereby only water pre-hydrolysis with or without the addition of foreign acid is used as pretreatment.
  • the acidity combined with the reaction temperature are the decisive factors of this pretreatment.
  • the addition of mineral acid reduces the time or the temperature required for the hydrolysis.
  • the acetyl groups of the hemicelluloses give rise to organic acids, in particular acetic acid, which causes the pH to drop to about 3-4 without the addition of acids.
  • acetic acid which causes the pH to drop to about 3-4 without the addition of acids.
  • the pH can drop further due to the high content of the acetyl groups.
  • mineral acids especially hydrochloric acid, accelerates the hydrolysis reaction, but has serious disadvantages, particularly with regard to corrosion and process costs.
  • the reaction conditions in the pre-hydrolysis influence the yield and the quality of the viscose pulp and they influence the delignification and the removal of further hemicelluloses when recondensation of lignins and of condensable reaction products of the hemicellulose hydrolysis takes place. This occurs in particularly harsh hydrolysis conditions in the pre-hydrolysis and in raw materials with a high lignin content, e.g. Conifers.
  • Water pre-hydrolysis sulfate viscose pulp from softwoods can reach alpha cellulose contents of 95-96% before bleaching, although it still contains approx. 3% lignin and 2-3% xylene.
  • Hardwoods generally contain more than 95% alpha cellulose, 1% lignin and 3-4% xylans.
  • the xylans are usually achieved by post-treatment with cold alkali during bleaching. However, this is a costly process step.
  • the pre-hydrolysis-sulfate process can open up all common raw materials for pulp production, achieves much higher alpha cellulose contents, a much more uniform molecular weight distribution of this cellulose and higher DP values.
  • the Sivola process is essentially an acidic sulfite digestion, followed by post-cleaning with hot sodium carbonate.
  • the following conditions are required for pulps with an alpha cellulose content and a purity comparable to that of the pre-hydrolysis-sulfate digestion: 170 ° C, 1-3 hours digestion time, in the alkaline step with sodium carbonate at a chemical dosage of 150-200 kg / t, to a pH of 9-9.5 to maintain, in addition 0.5-1% SO 2 must remain in the cellulose during the sodium carbonate boiling in order to achieve sufficient bleachability of the material.
  • the first stage is carried out at 125-135 ° C with a treatment time of 3 hours or more.
  • the pre-hydrolysis soda-anthraquinone boil is known longer than the sulfate boil, but could not prevail due to various cost and quality reasons.
  • the yield is low, the residual lignin content is relatively high, the purity is low and the DP of alpha cellulose is low.
  • 1.7 times more bleaching chemicals than chlorine are required than in the pre-hydrolysis sulfate process.
  • Another economic disadvantage is the addition of 0.5% anthraquinone. This chemical incurs significant additional costs.
  • the known methods for producing viscose pulp have different but serious disadvantages.
  • the pre-hydrolysis-sulfate processes can digest all common lignocelluloses, result in high-purity pulp with a high alpha cellulose content, which has a high uniformity in molecular weight and a high DP, but have the disadvantage of a low yield compared to the sulfite processes (28-30% compared to 30- 35%).
  • the production costs of viscose pulp are essentially determined by the raw material costs and the energy consumption. Another factor that determines the future is environmental compatibility. In various regions, there are already strict regulations regarding wastewater values, e.g. AOX, BOD, COD.
  • the object of the present invention is to develop an energy-saving process for the production of viscose pulp from the lignocelluloses customary for paper pulp production, which already has a high alpha-cellulose and low lignin content combined with high viscosity and yield values at the exit of the cooker, and its subsequent processing requires less technical effort and less bleaching chemicals in laundry, sorting and bleaching, as a result of which the process has significant product quality and cost advantages over conventional processes for the production of viscose pulp.
  • sulfite processes can only digest certain lignocelluloses, e.g. Wood types that are not common, such as pine, result in lower cellulose viscosity due to the required higher cooking temperature and acidity, the ⁇ -cellulose content does not reach more than 85-90% after a two-step boiling and only 95-96% after bleaching, the yield is only 29-35 % and the end product has limited use, for example not suitable for "high tenacity rayon cord".
  • Pre-hydrolysis is limited by the occurrence of side reactions that are difficult to control. In addition to the desired hydrolytic fragmentation reactions, secondary reactions occur which, depending on temperature and time, can have a lasting effect on the process behavior in pre-hydrolysis and the subsequent delignification reactions in digestion and bleaching. The most important side reaction The dehydration of the pentoses to furfural is the starting point for the undesirable inter- and intramolecular condensation reactions, resulting in resin-like compounds which, as the reaction continues, can separate from the aqueous phase and deposit on all existing surfaces.
  • the object of the invention is therefore also to overcome the problems associated with the undesirable by-products and the serious disadvantages of steam pre-hydrolysis on the end product quality, and to combine the energetic and procedural advantages of this process stage with an extended displacement boil that saves energy and bleaching chemicals.
  • the present invention accordingly relates to a process for the production of viscose pulp from lignocelluloses by a steam pre-hydrolysis sulfate (force) displacement cooking process, which is characterized in that after the pre-hydrolysis with saturated steam, the cooker with hot black liquor (HSL) is preceded by a boil and optionally also under The addition of fresh white liquor (WL) is filled and the hydrolysis products are neutralized, which results in the neutralizing liquor (NL) in the cooker that the amount of alkali required for the delignification in the cooking is supplied in the form of fresh white liquor (WL), with a partial amount of the NL if necessary is displaced that the cooking takes place with or without a temperature gradient and that the cooking is ended by displacing the cooking liquor (HSL) with alkaline washing filtrate (WF), whereby the alkali-soluble lignin of the pulped fiber material is washed out and the pulp for the discharge from the knockout cher is cooled.
  • HSL hot black liquor
  • FIG. 1 A preferred embodiment of the method in the form of a discontinuous process sequence is shown in FIG. 1.
  • a continuous process is possible or conceivable.
  • the process is divided into nine steps. The steam pre-hydrolysis and the cooking of the wood chips take place in one and the same cooker (KO).
  • At least four containers are required for the alkalis to neutralize the hydrolysis products of steam pre-hydrolysis and for subsequent boiling, namely for the hot white liquor (HWL) to adjust the required alkalinity of the alkalis for neutralization and cooking, and for the hot black liquor (HSL) from completed boilings , for the neutralization liquor (NL), which is formed by taking up the hydrolysis products of steam pre-hydrolysis from HSL and directly from the NL tank after heat recovery to the evaporation plant (EDA) and then to the caustic pot for chemical recovery and energy generation is carried out and for the alkaline washing filtrate (WF) from the brown cloth washing, with which the HSL is displaced from the cooker at the end of cooking and the temperature of the food is cooled to below 100 ° C.
  • the warm black liquor (WSL) that occurs at the end of the displacement of the HSL with WF is fed into a separate tank for heat recovery and subsequent transfer to the EDA.
  • the present invention is illustrated by Examples 1 and 2 below (see FIGS. 2 and 3).

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
EP94900624A 1992-12-02 1993-12-02 Verfahren zur herstellung von viskosezellstoffen Expired - Lifetime EP0672207B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT2382/92 1992-12-02
AT0238292A AT398588B (de) 1992-12-02 1992-12-02 Verfahren zur herstellung von viskosezellstoffen
PCT/AT1993/000183 WO1994012719A1 (de) 1992-12-02 1993-12-02 Verfahren zur herstellung von viskosezellstoffen

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Publication Number Publication Date
EP0672207A1 EP0672207A1 (de) 1995-09-20
EP0672207B1 true EP0672207B1 (de) 1996-11-06

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US (1) US5676795A (ru)
EP (1) EP0672207B1 (ru)
JP (1) JPH08503744A (ru)
CN (1) CN1041645C (ru)
AT (1) AT398588B (ru)
BR (1) BR9307589A (ru)
CA (1) CA2150381C (ru)
DE (1) DE59304443D1 (ru)
ES (1) ES2097021T3 (ru)
FI (1) FI952509A (ru)
RU (1) RU2122055C1 (ru)
WO (1) WO1994012719A1 (ru)

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US5183535B1 (en) * 1990-02-09 1996-02-06 Sunds Defibrator Rauma Oy Process for preparing kraft pulp using black liquor pretreatment reaction
US5213662A (en) * 1991-08-14 1993-05-25 Kamyr, Inc. Treatment of chips with high temperature black liquor to reduce black liquor viscosity

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016225827A1 (de) 2016-12-21 2018-06-21 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Zweistufiges Aufschlussverfahren zur chemischen Fraktionierung von Lignocellulose
WO2018114905A1 (de) 2016-12-21 2018-06-28 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Zweistufiges aufschlussverfahren zur chemischen fraktionierung von lignocellulose

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RU2122055C1 (ru) 1998-11-20
AT398588B (de) 1994-12-27
FI952509A0 (fi) 1995-05-23
CN1094108A (zh) 1994-10-26
JPH08503744A (ja) 1996-04-23
US5676795A (en) 1997-10-14
ATA238292A (de) 1994-05-15
CA2150381C (en) 2004-11-02
CN1041645C (zh) 1999-01-13
BR9307589A (pt) 1999-08-31
ES2097021T3 (es) 1997-03-16
RU95113599A (ru) 1997-05-27
CA2150381A1 (en) 1994-06-09
WO1994012719A1 (de) 1994-06-09
FI952509A (fi) 1995-05-23
EP0672207A1 (de) 1995-09-20
DE59304443D1 (de) 1996-12-12

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