EP1180171A1 - Verfahren zur herstellung von zellstoff, lignin, zucker und essigsäure durch fraktionierung des lignocellulosematerials mittels ameisensäure und essigsäure - Google Patents

Verfahren zur herstellung von zellstoff, lignin, zucker und essigsäure durch fraktionierung des lignocellulosematerials mittels ameisensäure und essigsäure

Info

Publication number
EP1180171A1
EP1180171A1 EP99916998A EP99916998A EP1180171A1 EP 1180171 A1 EP1180171 A1 EP 1180171A1 EP 99916998 A EP99916998 A EP 99916998A EP 99916998 A EP99916998 A EP 99916998A EP 1180171 A1 EP1180171 A1 EP 1180171A1
Authority
EP
European Patent Office
Prior art keywords
acetic acid
formic
mixture
paper pulp
sugars
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
Application number
EP99916998A
Other languages
English (en)
French (fr)
Other versions
EP1180171B1 (de
Inventor
Gérard Avignon
Michel Delmas
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.)
Industrielle de la Matiere Vegetale Cie
Original Assignee
CIE IND DES MATIERES VEGETALES
Industrielle des Matieres Vegetales Cie
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 CIE IND DES MATIERES VEGETALES, Industrielle des Matieres Vegetales Cie filed Critical CIE IND DES MATIERES VEGETALES
Publication of EP1180171A1 publication Critical patent/EP1180171A1/de
Application granted granted Critical
Publication of EP1180171B1 publication Critical patent/EP1180171B1/de
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
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • 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
    • D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment

Definitions

  • the invention relates to a process for the production of paper pulp, lignins, sugars and acetic acid from lignocellulosic plant material constituting most of the annual and perennial plants.
  • the papermaking quality of a pulp is defined in relation to the process of separation of cellulosic fibers or defibration and in relation to a series of physicochemical parameters, the most important of which are the length of break which translates the tensile strength, tear index and burst index. The higher these characteristics, the better the quality of the dough produced. We therefore consider:
  • thermomechanical which is obtained with a yield of around 80 to 90% by mechanical or thermomechanical processes
  • breaking length an essential characteristic of paper pulp and paper, corresponds to the length of a uniform strip of any width assumed to be suspended by one of its ends breaking under the effect of its own weight. This breaking length is calculated by formula 106. RT / 15 G. g in which:
  • - G is the grammage of the paper strip expressed in g / m2.
  • - g is the acceleration of gravity (9.81 m / s 2 ).
  • the processes for producing quality paper pulp are essentially chemical in nature in which the cellulosic fibers of the lignocellulosic plant material are freed from the vegetable cement, which binds them.
  • plants consisting of hemicelluloses (polymers of sugars with 5 or 6 carbons) and lignins (polymers of substituted allylic phenols) by a chemical action of hydrolysis in basic or acidic aqueous medium concentrated, often in the presence of sulfur in different oxidation states.
  • Formic acid B. BUCHOLZ and RK. JORDAN Pulp and Paper, p.102 - 104, 1983; MN. ERISMANN et al., Bioresource Technology, Vol. 47, p. 247 - 256, 1994
  • This technology also makes it possible to conserve the silica contained in the vegetable in paper pulp, which is an important advantage when annual plants are used as a raw material because silica disturbs considerably, in current industrial processes in basic medium. , recovery of mineral reagents.
  • MILOX process proceeds by formic acid cooking in several stages in the presence of hydrogen peroxide which improves delignification (K. POPPI US - LEVLIN et al. Tappi Journal, Vol. 80, N ° 9, p. 215-221, 1997).
  • Acetic acid can be used for the same purpose under pressure at higher temperature (160 to 180 ° C) at concentrations in water of 50 to 90% (RA YOUNG and JL DAVIS, Holzforshung, Vol. 40, p 99-108, 1986).
  • Delignification is correct, but the process requires washing the dough with acetone to remove the lignins precipitated from the dough.
  • a variant of this process makes it possible, with oxygen under pressure, to reduce cooking times and to improve delignification (CP NETO and A. ROBERT, Holzforshung, Vol. 46, p. 233-240, 1993), but it is at the origin of a partial depolymerization of cellulose by the joint action of pH and oxygen.
  • a variant of the MILOX process using two stages of cooking, acetic acid and hydrogen peroxide has also been proposed at 160-170 ° C (K. POPPIUS - LEVLIN et al., Paper and Timber, Vol. 73 p . 154-158, 1991), but it does not bring about any considerable improvement.
  • the present invention aims to propose a new process for manufacturing paper pulp from annual or perennial plants which leads to good quality chemical pulps retaining in their structure endogenous silica at atmospheric pressure.
  • the invention relates to a process which makes it possible to obtain these performances whatever the nature of the plants used and which is therefore particularly advantageous in the case of annual plants to open the way to new valuations, in particular in the case of cereal straws. and bagasse of sugar cane, or sugar sorghum.
  • the process for manufacturing paper pulp, lignins, sugars and acetic acid according to the invention is characterized in that it combines the following stages:
  • the solid fraction constituting the paste is then separated from the organic phase, containing in particular the starting formic and acetic acids, solubilized sugars and polymers, lignins and acetic acid derived from the initial vegetable raw material.
  • the process according to the invention results from the following surprising observation: the addition of acetic acid to formic acid makes it possible to considerably increase the solvating power of the liquid organic phase thus defined with respect to hemicelluloses and lignins without affect the acid hydrolysis capacity of these biopolymers by formic acid. In this way, the degradation of the cellulosic fibers which appears with the concentrated formic acid alone under the usual conditions of use is avoided, and the papermaking quality of the pulp obtained is therefore preserved.
  • Resistant pastes are then obtained which are easily separated from the reaction medium and which are easily dripped due to the non-salting out of endogenous silica.
  • This property is particularly important since it is the main limiting factor in the use of chemical straw pulp, especially in fast paper machines, the speed of which they slow down.
  • acetic acid preferably in molecular form, more easily dissolves lignins. thus released.
  • This effect makes it possible to limit the reaction time and the possible formylations of the free hydroxyl groups of the cellulose which degrade the paper qualities of the pulp.
  • the process according to the invention can be carried out from plants or parts of plants of the genus:
  • the humidity of the initial lignocellulosic material is less than or equal to 25% by weight of water relative to the dry material.
  • the lignocellulosic raw material is preferably ground so as to reduce it to fragments or shavings of length substantially between 0.5 and 20 cm.
  • the plant material is impregnated beforehand by at least 30 ° C. below the reaction temperature.
  • the impregnation by immersion is carried out for a period of 10 to 30 min in the formic acid / acetic acid mixture used during the fractionation reaction.
  • the impregnation and reaction of The following fractionation is carried out at atmospheric pressure.
  • fractionation is understood here to mean the reaction process usually known as baking which, under the conditions of the invention, leads, in addition to the paper pulp, to easily separable products, which is not the case. in most conventional methods.
  • the fractionation reaction is carried out at a temperature lower than or equal to the reflux temperature of the mixture.
  • the liquid / solid mass ratio will preferably be between 4 and 1 1.
  • the separation of the paper pulp from the organic phase at the end of cooking is preferably carried out by pressing.
  • Another preferred embodiment provides for the washing of the dough thus separated by a mixture of formic acid and acetic acid or pure acetic acid.
  • the dough, free of most of the lignin and sugar residues, is then washed with hot water.
  • Another preferred embodiment proceeds by cooking in at least two stages to improve delignification, and therefore the quality of the pasta.
  • the first step is carried out in the presence of the formic acid / acetic acid mixture.
  • the second stage is carried out after having separated the pulp produced in the first stage in the presence of anhydrous acetic acid.
  • the dough washes are carried out with acetic acid.
  • a preferred embodiment provides for pH control during washing in organic acid medium so that the paper pulp is at the ideal pH for bleaching with ozone in 1 or 2 sequences, at a dryness of the pulp. '' from 40 to
  • Another preferred embodiment provides for the separation of formic acid and acetic acid by vacuum evaporation, separation of entrained water, recycling of formic and acetic acids in the required proportions, and recovery of excess acetic acid and water.
  • Another mode of implementation provides for the lignin / sugar mixture taken up in water, the suspension is filtered or centrifuged to separate the precipitated lignins from the acidic aqueous sugar phase. The latter is concentrated by vacuum evaporation to recover the sugars and recycle the condensation water.
  • 38g of rice straw at 88% dryness (33.5g of dry matter) are brought into contact at room temperature (20 ° C) with a mixture containing 150g of pure formic acid and 150g of pure acetic acid in a reactor. 2 liters fitted with a central mechanical stirrer, an open cooler and a thermometer. The mechanical stirring is maintained for 15 min at ambient temperature which corresponds to the impregnation time.
  • the suspension is brought to the temperature of 100 ° C. by means of a thermostated heating bath in 35 min. This temperature is maintained in level for 60 min.
  • the dough is drained and separated by pressing, then washed twice in the reactor with 150 ml of a formic acid / acetic acid mixture in the proportions of the initial reaction for a period of 10 min.
  • the acidic washing solutions are separated from the paste by filtration and pressing, then the paste is washed with hot water to recover the traces of residual acids. The dough is then washed in cold water until neutral.
  • the mechanical characteristics of the dough obtained are as follows: GR (grammage): 72.35 g / m 2 NF standard: Q 03019
  • 38g of rice straw with 90% dryness (34.2g of dry matter) are brought into contact at room temperature (20 ° C) with a mixture containing 210g of pure formic acid and 90g of pure acetic acid in a reactor 2 liter tank fitted with a central mechanical stirrer, an open cooler and a thermometer. Mechanical stirring is maintained for 15 min at room temperature, which corresponds to the impregnation time.
  • the suspension is brought to the temperature of 85 ° C. by means of a heating bath thermostatically controlled in 25 min. This temperature is maintained in level for 60 min.
  • the dough is drained and separated by pressing, then washed twice in the reactor with 150 ml of a formic acid / acetic acid mixture in the proportions of the initial reaction for a period of 10 min.
  • the acidic washing solutions are separated from the dough by filtration and pressing, then the dough is washed with hot water and then with cold water.
  • the whiteness index measured using the ELREPHO 2000 spectrophotometer according to standard NFQ 03039 goes from 28.1 photovolts for raw pulp to 68.2 photovolts for pulp bleached under these conditions.
  • the mixture of formic and acetic acids obtained by evaporation of the sugar and lignin solution contains the water provided by the lignocellulosic raw materials.
  • This water is separated from the mixture of acids by azeotropic distillation using a third body which can be: ethyl acetate, benzene, toluene, n-butylethylether, cyclohexane, etc.
  • the separation of excess acetic acid from the acetyl groups of the lignocellulosic material can then be carried out by simple rectification.
  • 100 g of rice straw corresponding substantially to three identical tests under the experimental conditions described above provide approximately 10 g of water to the reaction medium.
  • the organic liquid phase contains substantially 880g of acetic and formic acids and 9.5g of water. It is treated with 109 g of ethyl acetate.
  • the ethyl acetate - water azeotrope (bp 70.4 ° C under 760 mm Hg, water concentration: 8.2% by weight) is extracted at the top of the column to be distilled and condensed.
  • the ethyl acetate is separated from the water in a decanter and it is recycled at the top of the column.
  • the dehydrated acetic acid / formic acid mixture is extracted at the bottom of column and can then be distilled in a rectification column to recover excess acetic acid.
  • the formic and acetic acids are then recycled to cooking in suitable proportions. After evaporation of the organic acids, the sugar and lignin mixture is treated with the water recovered during the washing of the dough.
  • Example No. 3 38g of sorghum bagasse with 88% dryness (33.5g of dry matter) are brought into contact at room temperature (20 ° C) with a mixture containing 220g of pure formic acid and 90g of acid pure acetic acid in a 2 liter reactor equipped with a central mechanical stirrer, an open cooler and a thermometer. The mechanical stirring is maintained for 30 min at ambient temperature which corresponds to the impregnation time.
  • the suspension is brought to the temperature of 100 ° C. by means of a heating bath thermostatically controlled in 30 min. This temperature is maintained in level for 60 min.
  • the paste is drained and separated by pressing then washed twice in the reactor with 150 ml of a formic acid / acetic acid mixture in the proportions of the initial reaction for a period of 10 min.
  • the acidic washing solutions are separated from the paste by filtration and pressing, then the paste is washed with hot water to recover the traces of residual acids.
  • the dough is then washed in cold water until neutral.
  • the pulp obtained is characterized by its degree of average viscosimetric polymerization (DPv).
  • the measurement is carried out using a capillary viscometer of the "Cellulose Commission” type which is used to determine the intrinsic viscosity (in mPa.s) of natural or regenerated cellulose (NF T 12-005).
  • DPv (0.75 (954 logv - 325)
  • 38g of rice straw with 88% dryness (33.5g of dry matter) are brought into contact at room temperature (20 ° C) with a mixture containing 220g of pure formic acid and 90g of pure acetic acid in a reactor 2 liter tank fitted with a central mechanical stirrer, an open cooler and a thermometer. Mechanical stirring is maintained for 15 min at room temperature which corresponds to the impregnation time.
  • the suspension is brought to the temperature of 100 ° C. by means of a heating bath thermostatically controlled in 30 min. This temperature is maintained in level for 60 min.
  • the dough is drained and separated by pressing.
  • the dough undergoes a second cooking with glacial acetic acid (150 ml) at a temperature of 90 ° C for 30 min.
  • the new paste obtained is drained, separated by pressing and washed three times with acetic acid (150 ml) for 15 min for each wash at a temperature of 95 ° C.
  • the acidic washing solutions are separated from the paste by filtration and pressing, then the paste is washed with hot water to recover the traces of residual acids. The dough is then washed in cold water until neutral.

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  • Paper (AREA)
  • Cereal-Derived Products (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)
EP99916998A 1999-05-06 1999-05-06 Verfahren zur herstellung von zellstoff, lignin, zucker und essigsäure durch fraktionierung des lignocellulosematerials mittels ameisensäure und essigsäure Expired - Lifetime EP1180171B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/FR1999/001071 WO2000068494A1 (fr) 1999-05-06 1999-05-06 Procede de production de pate a papier, lignines, sucres et acide acetique par fractionnement de matiere vegetale lignocellulosique en milieu acide formique/acide acetique

Publications (2)

Publication Number Publication Date
EP1180171A1 true EP1180171A1 (de) 2002-02-20
EP1180171B1 EP1180171B1 (de) 2003-10-08

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EP99916998A Expired - Lifetime EP1180171B1 (de) 1999-05-06 1999-05-06 Verfahren zur herstellung von zellstoff, lignin, zucker und essigsäure durch fraktionierung des lignocellulosematerials mittels ameisensäure und essigsäure

Country Status (8)

Country Link
US (1) US7402224B1 (de)
EP (1) EP1180171B1 (de)
AT (1) ATE251689T1 (de)
AU (1) AU3528699A (de)
DE (1) DE69912007T2 (de)
DK (1) DK1180171T3 (de)
ES (1) ES2209424T3 (de)
WO (1) WO2000068494A1 (de)

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WO2024184474A1 (fr) * 2023-03-08 2024-09-12 Rbx Creations Procédé d'obtention d'au moins deux pulpes cellulosiques présentant des caractéristiques différentes

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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.
FR2932815B1 (fr) * 2008-06-23 2015-10-30 Cie Ind De La Matiere Vegetale Cimv Procede de pretraitement de la matiere premiere vegetale pour la production, a partir de ressources sacchariferes et lignocellulosiques, de bioethanol et/ou de sucre, et installation.
AU2015203453B2 (en) * 2008-06-23 2016-09-22 Compagnie Industrielle De La Matiere Vegetale Cimv Method For Pretreating Plant Starting Material For The Production, From Sacchariferous And Lignocellulosic Resources, Of Bioethanol And Of Sugar, And Plant
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EP2336195A1 (de) * 2009-12-16 2011-06-22 Shell Internationale Research Maatschappij B.V. Verfahren zur Bearbeitung eines Lignozellulose-Biomassematerials
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FI123934B (en) * 2012-03-29 2013-12-31 Upm Kymmene Corp Use of low molecular weight lignin for the preparation of a binder composition
MX2014012867A (es) * 2012-04-26 2015-07-14 Archer Daniels Midland Co Separacion liquido / liquido de biomasa lignocelulosica para producir jarabes de azucar y fracciones de lignina.
FR2993568B1 (fr) 2012-07-17 2014-08-22 Compagnie Ind De La Matiere Vegetale Cimv Utilisation d'une lignine pour le renfort mecanique d'elastomeres, et elastomere ainsi renforce
CN103898786B (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
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
FR3007764B1 (fr) * 2013-06-26 2016-11-25 Cie Ind De La Matiere Vegetale - Cimv "resine phenolique obtenue par polycondensation de formaldehyde, de phenol et de lignine"
FR3021975B1 (fr) 2014-06-05 2018-03-30 Compagnie Industrielle De La Matiere Vegetale - Cimv Procede de production, notamment d'ethanol, par hydrolyse enzymatique sequencee de la cellulose et des hemicelluloses d'une matiere premiere lignocellulosique
SI3347307T1 (sl) 2015-09-09 2020-09-30 Compagnie Industrielle De La Matiere Vegetale Cimv Proces za ekstrakcijo silicijevega dioksida
DE102016219719B3 (de) * 2016-10-11 2018-01-25 Clariant International Ltd. Verfahren zur Gewinnung von Cellulose, Hemicellulose und Lignin aus Lignocellulose aus pflanzlicher Biomasse
DK3372646T3 (da) 2017-03-08 2020-10-19 Compagnie Ind De La Matiere Vegetale Cimv Fremgangsmåde til den samtidige ekstraktion af lignin og silika fra biomasse og elastomer forstærket med en blanding af lignin og silika
EP3527531A1 (de) * 2018-02-16 2019-08-21 Michel Delmas Auf lignocellulosebiomasse basierendes verfahren zur herstellung von ligninen und synthesegas und effizientes synthesegas zur elektrizitätserzeugung
EP3527608A1 (de) * 2018-02-16 2019-08-21 Michel Delmas Verfahren und kraftwerk zur bedarfsgerechten erzeugung von strom aus nicht-fossilen stromquellen und aus einem erneuerbaren lignocellulosehaltigen biomasse-rohstoff
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WO2024184474A1 (fr) * 2023-03-08 2024-09-12 Rbx Creations Procédé d'obtention d'au moins deux pulpes cellulosiques présentant des caractéristiques différentes
FR3146481A1 (fr) * 2023-03-08 2024-09-13 Rbx Creations Procédé d’obtention d’au moins deux pulpes cellulosiques présentant des caractéristiques différentes

Also Published As

Publication number Publication date
DE69912007D1 (de) 2003-11-13
DK1180171T3 (da) 2004-02-16
AU3528699A (en) 2000-11-21
ES2209424T3 (es) 2004-06-16
DE69912007T2 (de) 2004-06-24
US7402224B1 (en) 2008-07-22
WO2000068494A1 (fr) 2000-11-16
ATE251689T1 (de) 2003-10-15
EP1180171B1 (de) 2003-10-08

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