WO2012070072A2 - Procédé de production d'alpha-cellulose - Google Patents

Procédé de production d'alpha-cellulose Download PDF

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Publication number
WO2012070072A2
WO2012070072A2 PCT/IN2011/000816 IN2011000816W WO2012070072A2 WO 2012070072 A2 WO2012070072 A2 WO 2012070072A2 IN 2011000816 W IN2011000816 W IN 2011000816W WO 2012070072 A2 WO2012070072 A2 WO 2012070072A2
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WO
WIPO (PCT)
Prior art keywords
minutes
atleast
cellulose
pulp
range
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Application number
PCT/IN2011/000816
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English (en)
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WO2012070072A3 (fr
Inventor
Chinmay Mondal
Ramesh Shetar
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Godavari Biorefineries Limited
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Publication of WO2012070072A2 publication Critical patent/WO2012070072A2/fr
Publication of WO2012070072A3 publication Critical patent/WO2012070072A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/08—Fractionation of cellulose, e.g. separation of cellulose crystallites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00—Macromolecular compounds derived from lignocellulosic 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/12—Bleaching ; Apparatus therefor with halogens or halogen-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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/12—Bleaching ; Apparatus therefor with halogens or halogen-containing compounds
    • D21C9/14—Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with ClO2 or chlorites
    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/147—Bleaching ; Apparatus therefor with oxygen or its allotropic modifications
    • D21C9/153—Bleaching ; Apparatus therefor with oxygen or its allotropic modifications with ozone
    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/16—Bleaching ; Apparatus therefor with per compounds
    • D21C9/163—Bleaching ; Apparatus therefor with per compounds with peroxides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
    • D21H11/06—Sulfite or bisulfite pulp
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment

Definitions

  • the present invention relates to a process for obtaining alpha-cellulose. More particularly the present invention relates to a process for obtaining the alpha-cellulose with high molecular weight.
  • Cellulose is one of the few high volume renewable feedstocks used on a large scale by the chemical industry. Over 1.5 billion pounds of highly pure cellulose are used annually to produce food additives, fibers, paper and textiles. Recently, the cellulose is also used to produce the high end product such as specialty chemicals and plastics. Due to environment concerns the production of biodegradable products from cellulose is becoming popular. For producing biodegradable products for example plastic and polymerized derivatives, cellulose needs to be of requisite properties the most important ones are high purity and very high molecular weight.
  • the usual source of cellulose is lignocellulosic materials. There are number of processes which have been developed, by and large with the objective of producing cellulosic pulp suitable for use in the paper and textile industries. For such applications the important criteria for quality of cellulose include whiteness index, fibre length and strength of cellulose. However, these methods are not suitable for providing cellulose particularly alpha-cellulose with very high purity and having extremely high molecular weight.
  • the present invention is directed to provide a process for obtaining alpha-cellulose with high molecular weight and purity suitable for converting into biodegradable derivatives.
  • the present invention provides a process for obtaining alpha-cellulose comprising steps of:
  • the present invention is directed to provide an alpha-cellulose with very high molecular weight and purity suitable for converting alpha-cellulose into biodegradable derivatives.
  • the present invention provides alpha - cellulose of atleast 92% having high molecular weight in the range of 10,00,000-25,00,000
  • the present invention relates to the process for obtaining alpha-cellulose with high molecular weight and purity and the alpha-cellulose produced by the process of the present invention, with high molecular weight and purity suitable for converting into biodegradable derivatives for example plastics and polymers.
  • the present invention provides a process for obtaining alpha- cellulose with high molecular weight and purity in which process comprises:
  • lignocellulosic material includes any type of lignocellulosic material comprising cellulose, such as but not limited to non-woody-plant lignocellulosic material, wooden material, agricultural wastes, forestry residues, paper-production sludge, waste- water-treatment sludge, corn fiber from wet and dry mill corn ethanol plants, and sugar- processing residues.
  • the lignocellulosic material can include, but is not limited to, grass, selected from but not limiting to switch grass, cord grass, rye grass, reed canary grass, miscanthus, or a combination thereof; sugar-processing residues, selected from but not limited to sugar cane bagasse; agricultural wastes, selected from but not limited to rice straw, rice hulls, barley straw, corn cobs, wheat straw, canola straw, oat straw, oat hulls, and corn fiber; stover, selected from but not limited to soybean stover, corn stover; and forestry wastes, selected from but not limited to recycled wood pulp fiber, sawdust, hardwood, softwood, or any combination thereof.
  • Lignocellulosic materials are composed of mainly cellulose, hemicellulose, and lignin.
  • a lignocellulosic material on a dry basis, may contain about 50% (w/w) cellulose, about 30% (w/w) hemicellulose, and about 20% (w/w) lignin.
  • the lignocellulosic material can be of lower cellulose content, for example, containing 20% (w/w) cellulose.
  • the pretreatment of the lignocellulosic material may be carried out by subjecting the lignocellulosic raw material to a suitable step to dissociate the hemicellulose-cellulose-lignin complex and removing the hemicellulose.
  • the conventional treatment of lignocellulosic material includes acidic or basic hydrolysis.
  • Acids or bases used are strong acids and bases which unfortunately, promote undesirable side reactions such as lignin condensation and depolymerization of hemicellulose/cellulose causing cellulose degradation.
  • Cellulose degradation not only reduces the yield and quality of recovered pulp but it also creates the condition in which condensation of lignin with the products of cellulose degradation occurs, thereby degrading the quality of recovered fractions.
  • acidic or basic hydrolysis is carried out in presence of steam.
  • thermochemical process is described in Spanish patent ES87/6829, which uses steam at a temperature of 200-250 degree centigrade in a hermetically sealed reactor to treat previously ground lignocellulosic material. It is reported that the best results can be achieved with 210-240 degree centigrade for holding the material for 4-16 minutes. Other reported prehydrolysis temperature is between 155-170 degree centigrade and the hold time is 90-170 minutes. Thus, such acid hydrolysis steps are required to be carried out in presence of strong acids, at very high temperatures requiring very lengthy hold time making the process very costly due to high energy consumption and also further degrading the quality of the cellulose.
  • Other type of thermochemical treatment includes a sudden depressurization of the reactor, called steam explosion treatment. However, such known steam explosion treatment also requires very high cooking temperature, lengthy hold time and in some instances, the pretreatment protocol incorporates varying concentrations of a catalytic agent (e.g. acid).
  • a catalytic agent e.g. acid
  • the lignocellulosic material Prior to subjecting to the steam treatment, the lignocellulosic material may be subjected to a mechanical treatment, such as crushing, mashing or the like, thereby allowing the easy infiltration of steam and other chemicals during further processing into the cellulose raw materials and improving the desired effect to be achieved. Lignocellulosic material may also be saturated with water prior to subjecting to steam treatment to remove silica.
  • the pretreatment involves treating lignocellulosic raw material in contact with high pressure steam at temperature in the range 190°C - 200°C for atleast 2 minutes for hydrolyzing and solubilizing the hemicellulose, separating the solubilized hemicellulose and washing the undissolved fibrous organic biomass with hot soft water to give the pretreated lignocellulosic material.
  • the evaporation (concentrating) of the water from the solubilized hemicellulose fraction gives the Hemicellulose, It was surprisingly found that very short hold time of 2-4 minutes was enough for the requisite separation of hemicellulose and provided desired quality of pre-treated material.
  • the percentage of hemicellulose separated in the form of xylans is in the range of about 18-22% on weight basis.
  • the pretreated lignocellulosic material is subjected to pulping by cooking the pre-treated pulp with sodium sulfite Na2So 3 , Sodium carbonate Na2C0 3 and Sodium Hydroxide (NaOH) in presence of anthraquinone at temperatures in the range 125- 180 ° C for atleast 15 minutes, preferably for 15-45 minutes to solubilize all the lignin component mainly into lignosulfonates.
  • the cooked pulp is then washed with water to remove adhering lignosulfonates and other impurities. Such washed and cooked pulp is screened to remove shives.
  • the lignosulfonates obtained after separating cooked pulp can be in the range of 16-18 % on weight basis.
  • the sodium sulfite (Na 2 S0 3 ) may be employed in an amount of about 5% - 25% as Na 2 0, preferably, 10% - 15% by weight.
  • Sodium carbonate (Na 2 C0 3 ) may be employed in the range of about 0.1% - 10% as Na 2 0, preferably 0.5% - 5% by weight.
  • Sodium Hydroxide (NaOH) may be used in the range of about 0.25% - 15% as Na 2 0, preferably in the range of about 0.5% - 5% by weight.
  • Anthraquinone may be employed in the range of about 0.01% - 0.3%, preferably in the range of about 0.01% to 0.2% by weight.
  • the bleaching of pulp is carried out.
  • the residual lignin is a major contributing factor as an impurity, hence it must be removed.
  • the chemicals used in bleaching in the process of the present invention effectively remove residual lignin and also dissolved extractives contained in the pulp (e.g. resin).
  • the bleaching of the pulp is carried out in multiple steps and the pulp is washed between them.
  • the Multi-step bleaching gives the best results regarding both quality and economy and it also addresses environment concerns over chlorinated organic by products from elemental chlorine and its derivatives. Due to such multi-stage bleaching process the AOX (Adsorable organic hallide) load can be achieved around 0.5 kg/BDMT of pulp and it also helps to achieve the better pulp properties.
  • the multi-step bleaching comprises of following steps carried out under defined conditions of temperature, pH and time duration: i) treating the washed pulp obtained from pulping step with active bleaching agent, followed by washing; ii) treating the washed pulp of (i) with alkali and washing; iii) treating the washed pulp of (ii) with active bleaching agent and washing.
  • the active bleaching agent that may be used may be selected from the group consisting of but not limited to chlorine dioxide, hypochlorite, sodium chlorite, hydrogen peroxide, ozone or the like.
  • the alkali used may be sodium hydroxide.
  • concentrations of the active bleaching agent and alkali to be employed in the above step (i) to (iii) may be about 0.1% -10 %, preferably active bleaching agent may be about 2% - 5% by weight and alkali may be about 3% -5% by weight.
  • the above bleaching steps are carried out under various conditions of temperature, pH and for a desired time duration.
  • the temperature in step (i) may be atleast 50 degree centigrade and in step (ii) and step (iii) the temperature may be atleast 70 degree centigrade.
  • the duration for which the step (i) may be carried out is atleast 30 minutes, preferably about 30 minutes to 60 minutes, step (ii) may be carried out for the duration of atleast 60 minutes, preferably about 60 minutes to 120 minutes and step (iii) may be carried out for atleast 90 minutes, preferably about 150 minutes to 180 minutes.
  • the pH in step (i) may be atleast 2, in step (ii) it may be atleast 10 and in step (iii) it may be atleast 3.
  • the yield of alpha - cellulose obtained is atleast 30%, preferably more than 35%.
  • the alpha- cellulose obtained by the process of the present invention has high purity of atleast 92%.
  • the molecular weight of the alpha - cellulose obtained is very high in the range of 10,00,000-25,00,000.
  • Hereto followed processes have not known to achieve such high yield, purity and particularly high molecular weight of alpha-cellulose suitable for conversion into cellulose derivatives for biodegradable materials for example plastics and polymers.
  • Alpha-cellulose with high molecular weight and purity can be readily converted into high end products like biodegradable cellulose derivatives for example plastics and other polymeric materials. Additionally, hemicellulose (xylan) 18 -22 % and 16-18 % lignosulfonates obtained by the process of the present invention can be further converted into industrially useful products, rendering the process commercially cost effective.
  • the process according to the present invention is extremely useful for effective utilization of natural resources and waste material and converting them into high demand high value commodities.
  • a 4.8 Kg of the steam exploded material was pulped by cooking with 1.3 kg sodium sulfite, 0.211 kg sodium carbonate, 0.082 Kg sodium hydroxide and 10 grams anthraquinone in 500 K L Hastelloy reactor for about 30 minutes and temperature of about 160 degree.
  • the cooked pulp was washed well with hot soft water.
  • the filtrate contained 1.1 Kg lignosulfonates.
  • Washed cooked pulp was screened to remove shives 2.43 Kg pulp obtained after screening was bleached with 31 gm sodium chlorite in first stage for 60 minutes at 60 degree centigrade at pH 2.6, followed by alkali extraction with 58 gm sodium hydroxide for 120 minutes, at temperature 70 degree centigrade at pH 10.9 and treatment with 12 gm sodium chlorite for 180 minutes, at 70 degree centigrade, at pH 3.2 in subsequent stage. The final bleached pulp was air dried. The final cellulose pulp obtained was 2.4 kg with 85 % brightness (Photo Volt) and alpha cellulose content of 94 % with molecular weight of 21,00,000.
  • a 9.4 Kg of the steam exploded material was pulped by cooking with 2.561 kg sodium sulfite, 0.419 kg sodium carbonate, 0.163 Kg sodium hydroxide and 25 grams anthraquinone in 500 K L Hastelloy reactor for about 30 minutes and temperature of about 160 degree.
  • the cooked pulp was washed well with hot soft water.
  • the filtrate contained 25 Kg I ignosulfonates.
  • Washed cooked pulp was screened to remove shives 4.70 Kg pulp obtained after screening was bleached with 68 gm sodium chlorite in first stage for 60 minutes at 60 degree centigrade at pH 2.8, followed by alkali extraction with 94 gm sodium hydroxide for 120 minutes, at temperature 70 degree centigrade at pH 11.1 and treatment with 28 gm sodium chlorite for 180 minutes, at 70 degree centigrade, at pH 3.2 in subsequent stage.
  • the final bleached pulp was air dried.
  • the final cellulose pulp obtained was 4.8 kg with 88 % brightness (Photo Volt) and alpha cellulose content of 94.3 % with molecular weight of 22,00,000.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

La présente invention concerne une alpha-cellulose de haut poids moléculaire et de haute pureté ainsi qu'un procédé de production de ladite alpha-cellulose à partir de matière lignocellulosique. La matière première lignocellulosique est traitée par mise en contact de celle-ci avec de la vapeur haute pression à une température comprise entre 190 °C et 200 °C pendant au moins 2 minutes pour permettre la solubilisation de la fraction hémicellulosique. La biomasse organique fibreuse non dissoute est lavée à l'eau douce chaude pour permettre l'obtention de la matière lignocellulosique prétraitée. La matière lignocellulosique prétraitée est réduite en pâte à l'aide de sulfite, d'alcali et d'anthraquinone à une température d'au moins 120 °C avec une durée de maintien d'au moins 15 minutes pour permettre la solubilisation de la lignine constituant la matière, par transformation en lignosulfonate. La pâte lavée et épurée est blanchie et lavée pour permettre d'obtenir la pâte contenant au moins 92 % d'alpha-cellulose de haut poids moléculaire compris entre 1 000 000 et 2 500 000. Une telle alpha-cellulose de haut poids moléculaire et de haute pureté est appropriée pour la transformation en dérivés biodégradables.
PCT/IN2011/000816 2010-11-26 2011-11-28 Procédé de production d'alpha-cellulose WO2012070072A2 (fr)

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IN3240MU2010 2010-11-26
IN3240/MUM/2010 2010-11-26

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WO2012070072A2 true WO2012070072A2 (fr) 2012-05-31
WO2012070072A3 WO2012070072A3 (fr) 2016-05-26

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105001457A (zh) * 2015-06-24 2015-10-28 济南圣泉集团股份有限公司 一种吸音降噪助剂
WO2015200868A1 (fr) * 2014-06-27 2015-12-30 Inventure Renewables, Inc. Procédés de production d'une pâtes d'alpha-cellulose à pureté élevée
WO2017044030A1 (fr) * 2015-09-07 2017-03-16 Domsjö Fabriker Ab Nouvelle pâte de dissolution
WO2017029685A3 (fr) * 2015-08-19 2017-05-11 Godavari Biorefineries Limited Procédé de production de cellulose présentant de faibles impuretés à partir de bagasse de canne à sucre
CN110731360A (zh) * 2019-10-10 2020-01-31 广西科技师范学院 一种食品级微晶纤维素的制备方法及其应用
EP3885488A4 (fr) * 2018-12-31 2022-01-19 Unicharm Corporation Procédé de production de matière première de fibre de pâte, et matière première de fibre de pâte en tant que matière première de cellulose

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5139617A (en) * 1987-04-21 1992-08-18 Suomen Sokeri Oy Process for the production of a hemicellulose hydrolysate and special high alpha cellulose pulp
JP2002537503A (ja) * 1999-02-24 2002-11-05 エスシーエー ハイジーン プロダクツ ゲゼルシャフト ミト ベシュレンクテル ハフツング 酸化されたセルロース含有繊維材料及びそれから作られた製品
EP1215217A1 (fr) * 2000-12-12 2002-06-19 SCA Hygiene Products Zeist B.V. Cellulose oxydée à poids moléculaire élevé

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015200868A1 (fr) * 2014-06-27 2015-12-30 Inventure Renewables, Inc. Procédés de production d'une pâtes d'alpha-cellulose à pureté élevée
CN105745377A (zh) * 2014-06-27 2016-07-06 因温特国际有限公司 生产高α-纤维素纸浆的方法
US10927497B2 (en) 2014-06-27 2021-02-23 Inventure Renewables Inc. Methods for the production of high alpha-cellulose pulp
CN105001457A (zh) * 2015-06-24 2015-10-28 济南圣泉集团股份有限公司 一种吸音降噪助剂
WO2017029685A3 (fr) * 2015-08-19 2017-05-11 Godavari Biorefineries Limited Procédé de production de cellulose présentant de faibles impuretés à partir de bagasse de canne à sucre
US10954630B2 (en) 2015-08-19 2021-03-23 Godavari Biorefineries Ltd. Process for producing cellulose with low impurities from sugarcane bagasse
WO2017044030A1 (fr) * 2015-09-07 2017-03-16 Domsjö Fabriker Ab Nouvelle pâte de dissolution
EP3885488A4 (fr) * 2018-12-31 2022-01-19 Unicharm Corporation Procédé de production de matière première de fibre de pâte, et matière première de fibre de pâte en tant que matière première de cellulose
CN110731360A (zh) * 2019-10-10 2020-01-31 广西科技师范学院 一种食品级微晶纤维素的制备方法及其应用

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