WO2014109345A1 - Composition de biomasse pour saccharification, procédé de sélection de composition de biomasse pour saccharification, et procédé de production de sucre - Google Patents

Composition de biomasse pour saccharification, procédé de sélection de composition de biomasse pour saccharification, et procédé de production de sucre Download PDF

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Publication number
WO2014109345A1
WO2014109345A1 PCT/JP2014/050181 JP2014050181W WO2014109345A1 WO 2014109345 A1 WO2014109345 A1 WO 2014109345A1 JP 2014050181 W JP2014050181 W JP 2014050181W WO 2014109345 A1 WO2014109345 A1 WO 2014109345A1
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Prior art keywords
saccharification
biomass
biomass composition
cellulose
mass
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PCT/JP2014/050181
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English (en)
Japanese (ja)
Inventor
若林　正一郎
藤田　一郎
米田　正
遠藤　貴士
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昭和電工株式会社
独立行政法人産業技術総合研究所
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Publication of WO2014109345A1 publication Critical patent/WO2014109345A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00—Sugars not otherwise provided for in this class
    • C13K13/002—Xylose
    • 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
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials

Definitions

  • the present invention relates to a biomass composition for saccharification having improved saccharification performance suitable as a reaction raw material in a method for producing sugar by hydrolysis of cellulose-containing biomass, a method for selecting the same, and a method for producing sugar.
  • cellulose-containing biomass examples include hard biomass such as cedar and cypress, and soft biomass such as rice straw, straw, corn cob, cassava, bagasse and sugarcane leaves. Since these biomasses may contain hemicellulose, lignin and the like and are difficult to saccharify as they are, proposals have been made to improve saccharification performance by various pretreatments.
  • Acid treatment is a technology that can effectively remove hemicellulose, an impurity, but it is necessary to neutralize the equipment corrosion due to acid and the acid used in the post-process, which increases costs when implemented industrially.
  • Alkali treatment is a technique that can effectively remove lignin, which is an impurity, but has a problem that the cost is high when it is industrially implemented because the loss of cellulose is large and the basic unit deteriorates.
  • Non-Patent Document 1 In addition to the above, steam explosion, ammonia explosion, ozone oxidation, white rot treatment, microwave irradiation, electron beam irradiation, and ⁇ -ray irradiation have been proposed (Non-Patent Document 1). However, these are treatment methods that require equipment costs and chemical costs, and are insufficient for industrial implementation from the viewpoint of cost effectiveness.
  • An object of the present invention is to provide a saccharification biomass composition with improved saccharification performance suitable as a reaction raw material in a saccharide production method by hydrolysis reaction of cellulose-containing biomass, a method for selecting the saccharification biomass composition, and a saccharide production method. Is to provide.
  • the saccharification biomass composition containing cellulose has not only a large specific surface area but also a low hemicellulose content in the composition. It has been found that a saccharification biomass composition that is high, that is, contains cellulose, has a specific surface area of 150 to 600 m 2 / g in a dry state, and has a hemicellulose content of 1 to 15% by mass, has high saccharification performance, The present invention has been completed.
  • the present invention relates to the following saccharification biomass composition, a method for selecting a saccharification biomass composition, and a method for producing sugar.
  • a biomass composition for saccharification comprising cellulose, having a specific surface area in a dry state of 150 to 600 m 2 / g, and a hemicellulose content in a dry state of 1 to 15% by mass.
  • the biomass composition for saccharification according to item 1 wherein the specific surface area is 150 to 300 m 2 / g.
  • the biomass composition for saccharification according to item 1 or 2 wherein the specific surface area is 150 to 200 m 2 / g.
  • a method for selecting a biomass composition for saccharification containing cellulose, wherein a composition having a specific surface area in a dry state of 150 to 600 m 2 / g and a hemicellulose content of 1 to 15% by mass is selected A method for selecting a biomass composition for saccharification characterized by the above.
  • Efficiency is obtained when a biomass composition for saccharification containing cellulose, having a specific surface area in a dry state of 150 to 600 m 2 / g, and having a hemicellulose content of 1 to 15% by mass is used as a method for producing sugar by hydrolysis reaction.
  • Sugar can be produced well.
  • the biomass composition for saccharification in the present invention has a specific surface area in a dry state of 150 to 600 m 2 / g, preferably 150 to 300 m 2 / g, more preferably 150 to 200 m 2 / g.
  • Production of a composition having a specific surface area exceeding 600 m 2 / g is expensive in terms of industrial production, and a composition having a specific surface area of less than 150 m 2 / g is reduced in saccharification performance, resulting in an increase in sugar production cost.
  • the specific surface area is measured by a BET method using nitrogen gas.
  • the biomass composition for saccharification in the present invention has a hemicellulose content in a dry state of 1 to 15% by mass, preferably 4 to 12% by mass, and more preferably 6 to 10% by mass.
  • a composition having a hemicellulose content of more than 15% by mass has a low saccharification performance, resulting in a high sugar production cost.
  • Production of a composition having a hemicellulose content of less than 1% by mass has an expensive industrial production cost.
  • the total content of lignin and ash is preferably 10 to 60% by mass, more preferably 15 to 55% by mass, and still more preferably 20 to 50% by mass.
  • the productivity per volume of the saccharification reaction tank decreases, so that the production cost becomes expensive, and the total content of lignin and ash is less than 10% by mass. Production is expensive due to industrial manufacturing costs.
  • the crystallinity of cellulose is preferably 1 to 60%, more preferably 5 to 50%, and still more preferably 11 to 40%.
  • the crystallinity of the cellulose exceeds 60%, the saccharification performance decreases, so that the sugar production cost becomes expensive.
  • the cellulose crystallinity is less than 1%, the production of the composition makes the industrial production cost expensive.
  • the biomass composition for saccharification in the present invention is preferably obtained by pretreating cellulose-containing biomass.
  • Biomass in the present invention means industrial resources originating from biopolymers (nucleic acids, proteins, polysaccharides) and their constituent elements, excluding exhaustible resources (fossil fuels such as oil, coal, and natural gas).
  • examples of the cellulose-containing biomass include hard biomass such as wood, and soft biomass such as rice straw, straw, corn cob, cassava, bagasse, and sugarcane leaves.
  • Soft biomass is preferable in consideration of ease of pretreatment, and bagasse and sugarcane leaves are particularly preferable in consideration of the global abundance and collection costs.
  • pulverize the cellulose-containing biomass that is the raw material of the biomass composition for saccharification before pretreatment.
  • pulverization it is preferable to separate the pulverized product using a screen (sieve) having a screen diameter of 1 to 30 mm ⁇ .
  • a more preferable range of the screen diameter is 2 to 20 mm ⁇ , and a most preferable range is 3 to 10 mm ⁇ . If the screen diameter when pulverizing is too large, the particle size of the cellulose-containing biomass will be large and the subsequent pretreatment effect will be low, resulting in high sugar production costs. Becomes expensive.
  • the pulverizer When pulverizing without using a screen, it is preferable to pulverize to a size corresponding to the pulverized product using the screen.
  • the pulverizer that can be used include a uniaxial pulverizer, a biaxial pulverizer, an extruder, a pelletizer, a roller mill, and a refiner.
  • the pretreatment of the cellulose-containing biomass in the present invention is preferably performed by pulverizing the hydrothermal treatment heated to 180 to 250 ° C. in the presence of water and the hydrothermally treated cellulose-containing biomass.
  • airtight containers such as an autoclave
  • the heating temperature during the hydrothermal treatment is more preferably 190 to 240 ° C, and most preferably 200 to 230 ° C.
  • the heating temperature is too high, not only the energy cost is increased, but also the decomposition of cellulose and the excessive decomposition of impurities proceed. On the other hand, if the heating temperature is too low, the pretreatment effect is lowered, and the sugar production cost becomes expensive.
  • the heating time in the hydrothermal treatment is preferably 1 to 100 minutes. More preferably, it is 2 to 30 minutes, and most preferably 3 to 15 minutes. If the heating time is too long, the productivity in the pretreatment process is lowered, so that the sugar production cost becomes expensive. If the heating time is too short, the pretreatment effect is lowered, and the sugar production cost is expensive. In addition, the preferable range of said heating time changes in said range with the heating temperature implemented.
  • the ratio of the cellulose-containing biomass to water in the hydrothermal treatment is preferably 4 to 97 times the amount of water with respect to the dry mass of the cellulose-containing biomass.
  • the amount is more preferably 6 to 20 times, and most preferably 8 to 13 times. If the amount of water relative to the dry mass of the cellulose-containing biomass is too large, the scale of the pretreatment device will be large and not economical, and if the amount of water relative to the dry mass of the cellulose-containing biomass is too small, the pretreatment effect will be low. As a result, the production cost of sugar becomes high.
  • the pretreatment of the cellulose-containing biomass in the present invention is advantageously heated in the presence of water, but it is also possible to add an acid or an alkali as an additive.
  • an acid or an alkali as an additive.
  • the use of additives not only incurs the cost of the drug, but also incurs costs for detoxification such as neutralization in the post-process, so it is most preferable to use only water that is generally available industrially. .
  • a biomass composition for saccharification by hydrolyzing the cellulose-containing biomass and then finely pulverizing it multiple times.
  • the number of times of pulverization is preferably 4 to 50 times, more preferably 6 to 30 times. If the number of fine pulverizations is too small, the pretreatment effect is lowered and the sugar production cost becomes expensive.
  • an apparatus for pulverization an apparatus using an impact force, a compressive force, a shear force, and a combination thereof is known.
  • a compressive force and a shear force are used in order to unwind cellulose fibers and improve a specific surface area.
  • a pulverizing apparatus utilizing the above is preferable. Specifically, a refiner, a disk mill, etc. are illustrated. The above effects cannot be sufficiently exhibited by a pulverization method such as a ball mill, a stamp mill, or a cutter mill.
  • each sample is introduced between plates or discs and pulverized. At that time, the longer the sample stays between the plates or disks, the higher the fine grinding effect. For this reason, as a shape of a plate or a disk, the structure which does not have the flow path penetrated in the circumferential direction from the center is preferable.
  • the flow path referred to here is a space formed between the cutting blades formed on the plate.
  • the method for selecting a biomass composition for saccharification according to the present invention is a method for selecting a saccharification biomass composition according to the present invention that satisfies the above conditions. By implementing the selection method from the viewpoint, a good biomass composition for saccharification can be obtained.
  • the hydrolysis method for saccharifying the obtained biomass composition for saccharification include a cellulose hydrolysis method using a solid acid catalyst and a mineral acid catalyst such as sulfuric acid, and an enzyme cellulose hydrolysis method.
  • the enzymatic hydrolysis method is industrially advantageous because it produces less impurities and the utility value of the resulting sugar is high.
  • the enzymatic hydrolysis of cellulose is performed, for example, by allowing a generally known cellulase to act on the biomass composition for saccharification according to the present invention.
  • a generally known cellulase to act on the biomass composition for saccharification according to the present invention.
  • the properties of cellulase vary slightly depending on the type, the optimum pH range is 3.5 to 5.5 and the optimum temperature range is 35 to 55 ° C.
  • cellulose can be hydrolyzed to produce sugar.
  • Method for analyzing cellulose content and hemicellulose content 300 mg of biomass dried at 105 ° C. for 1 hour was weighed into a 100 ml screw mouth reagent bottle. Thereto was added 3 ml of 72% sulfuric acid, and the mixture was thoroughly stirred with a glass rod and treated in a thermostatic bath at 30 ° C. for 1 hour. During the treatment in the constant temperature layer, it was occasionally stirred with a glass rod. After completion of the treatment, 84 ml of pure water was added, and the screw cap was loosely covered, followed by treatment at 121 ° C. for 1 hour in a sterilization autoclave (Tomy Industries, Ltd., SS-240).
  • the treatment liquid was subjected to suction filtration using a nitrocellulose filter, and the mass (A) of the filtrate was measured. A portion of the filtrate was taken, neutralized with calcium carbonate, filtered, and subjected to high-performance liquid chromatography analysis to quantify glucose produced by hydrolysis of cellulose and xylose produced by hydrolysis of hemicellulose (xylan).
  • This washing with t-butanol was repeated 40 times.
  • the washed sample was freeze-dried at room temperature for 1 week using a freeze-dryer (Tokyo Rika Kikai Co., Ltd., FDU-2100). This freeze-dried sample was used as a sample for XRD measurement and specific surface area measurement.
  • Mecerase registered trademark, cellulase manufactured by Meiji Seika Pharma Co., Ltd.
  • 98.5 g of pure water 1.5 g of Mecerase (registered trademark, cellulase manufactured by Meiji Seika Pharma Co., Ltd.) was dissolved in 98.5 g of pure water.
  • Saccharification reaction Put the rotor in a 50 ml lidded glass container, weigh the pretreatment composition so that the cellulose content is 0.5 g, add 0.6 g of the above acetate buffer and 1.03 g of enzyme solution, and then add pure water. The total amount was 10 g.
  • the enzymatic saccharification reaction was carried out for 48 hours while stirring in a 40 ° C. constant temperature bath. The obtained saccharified solution was subjected to high performance liquid chromatography analysis to quantify glucose, and the saccharification rate was determined.
  • Example 1 Sugarcane leaves were pulverized with a cutter mill (Masuyuki Sangyo Co., Ltd., MKCM-3, 3 mm ⁇ screen). The water content of the sugarcane leaves after pulverization was 10.4% by mass. 447 g of this sugarcane leaf was placed in a 10 liter autoclave (Desktop Reactor OML-10 manufactured by OM Lab Tech Co., Ltd.). Further, 3953 g of pure water was added, and the autoclave was sealed. While stirring at 500 rpm, the temperature controller of the liquid temperature was set to 200 ° C. and heating was started. Heating was continued for 10 minutes after the liquid temperature reached 190 ° C., and then heating was stopped and cooling was performed.
  • a cutter mill Mosuyuki Sangyo Co., Ltd., MKCM-3, 3 mm ⁇ screen.
  • the water content of the sugarcane leaves after pulverization was 10.4% by mass. 447 g of this sugarcane leaf was placed in
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter (manufactured by Kokusan Co., Ltd., H-122, filter cloth cotton) to obtain a water-containing solid content.
  • a centrifugal filter manufactured by Kokusan Co., Ltd., H-122, filter cloth cotton
  • Water was added so that the solid content concentration was 5% by mass, and wet pulverization was performed 10 times with a super mass colloider (manufactured by Masuko Sangyo Co., Ltd., MKCA6-2, disk MKG-C6-120) at a 1200 rpm clearance of 200 ⁇ m.
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained water-containing solid content has a specific surface area of 171 m 2 / g in a dry state, a hemicellulose content of 9.0% by mass, a total content of lignin and ash of 33.5% by mass, and a crystallinity of cellulose of 28%.
  • the saccharification rate after 48 hours was 79%.
  • Example 2 Sugarcane leaves were crushed with a cutter mill. The water content of the sugarcane leaves after pulverization was 10.4% by mass. 447 g of this sugarcane leaf was placed in a 10 liter autoclave. Further, 3949 g of pure water and 4.1 g of sulfuric acid were added, and the autoclave was sealed. While stirring at 500 rpm, the temperature controller of the liquid temperature was set to 200 ° C. and heating was started. Heating was continued for 10 minutes after the liquid temperature reached 190 ° C., and then heating was stopped and cooling was performed. The obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained water-containing solid content had a specific surface area of 155 m 2 / g, a hemicellulose content of 4.6% by mass, a total content of lignin and ash of 32.9% by mass, and a crystallinity of cellulose of 21%.
  • the saccharification rate was 72%.
  • Comparative Example 1 Sugarcane leaves were crushed with a cutter mill. The water content of the sugarcane leaves after pulverization was 10.6% by mass. 447 g of this sugarcane leaf was placed in a 10 liter autoclave. Further, 3953 g of pure water was added, and the autoclave was sealed. While stirring at 500 rpm, the temperature controller of the liquid temperature was set to 150 ° C. and heating was started. After the liquid temperature reached 142.5 ° C., the heating was continued for 240 minutes, and then the heating was stopped to cool. The obtained slurry was wet pulverized 10 times with a super mass collider at 1800 rpm clearance of 200 ⁇ m.
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained water-containing solid content has a specific surface area of 150 m 2 / g, hemicellulose content of 16.9% by mass, lignin and ash content of 26.2% by mass, cellulose crystallinity of 22%, and 48 hours later.
  • the saccharification rate was 61%.
  • Comparative Example 2 Sugarcane leaves were crushed with a cutter mill. The water content of the sugarcane leaves after pulverization was 10.6% by mass. 447 g of this sugarcane leaf was placed in a 10 liter autoclave. Further, 3953 g of pure water and 80 g of sodium sulfite were added, and the autoclave was sealed. While stirring at 500 rpm, the temperature controller of the liquid temperature was set to 150 ° C. and heating was started. After the liquid temperature reached 142.5 ° C., the heating was continued for 240 minutes, and then the heating was stopped to cool. The obtained slurry was wet pulverized 10 times with a super mass collider at 1800 rpm clearance of 200 ⁇ m.
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained water-containing solid content was a specific surface area of 220 m 2 / g, a hemicellulose content of 23.1% by mass, a total content of lignin and ash of 8.8% by mass, and a crystallinity of cellulose of 25%.
  • the saccharification rate was 56%.
  • Comparative Example 3 Sugarcane leaves were crushed with a cutter mill. The water content of the sugarcane leaves after pulverization was 10.4% by mass. 447 g of this sugarcane leaf was placed in a 10 liter autoclave. Further, 3953 g of pure water was added, and the autoclave was sealed. While stirring at 500 rpm, the temperature controller of the liquid temperature was set to 200 ° C. and heating was started. Heating was continued for 10 minutes after the liquid temperature reached 190 ° C., and then heating was stopped and cooling was performed. The obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained slurry was subjected to centrifugal filtration at 3000 rpm using a centrifugal filter to obtain a water-containing solid content.
  • the obtained water-containing solid content was a specific surface area of 137 m 2 / g, a hemicellulose content of 4.8% by mass, a total content of lignin and ash of 32.5% by mass, and a crystallinity of cellulose of 29%.
  • the saccharification rate was 57%.

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Abstract

L'invention concerne une composition de biomasse pour saccharification, convenant en tant que matériau brut de réaction utilisée dans un procédé de production de sucre au moyen d'une réaction d'hydrolyse de biomasse contenant une cellulose, et présentant une performance de saccharification améliorée. L'invention concerne également un procédé de sélection de composition de biomasse pour saccharification ; et un procédé de production de sucre consistant à hydrolyser la composition de biomasse pour saccharification. Selon l'invention, la composition de biomasse pour saccharification contient une cellulose, comprend une zone de surface spécifique de 150 à 600 m2/g à l'état sec et une teneur en hémicellulose de 1 à 15 % en masse, et contient de la lignine et une teneur en cendres de 10 à 60 %, en masse de la quantité totale, la cellulose présentant un degré de cristallinité de 1 à 60 %.
PCT/JP2014/050181 2013-01-10 2014-01-09 Composition de biomasse pour saccharification, procédé de sélection de composition de biomasse pour saccharification, et procédé de production de sucre WO2014109345A1 (fr)

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JP2013-002601 2013-01-10

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006136263A (ja) * 2004-11-12 2006-06-01 National Institute Of Advanced Industrial & Technology リグノセルロース系バイオマス処理方法
JP2006141244A (ja) * 2004-11-17 2006-06-08 National Institute Of Advanced Industrial & Technology リグノセルロースの糖化方法及びそれによって得られた糖
JP2007282597A (ja) * 2006-04-19 2007-11-01 Ihi Corp 木質バイオマスの可溶化方法
JP2008271962A (ja) * 2007-04-04 2008-11-13 National Institute Of Advanced Industrial & Technology 糖の製造方法
WO2009096061A1 (fr) * 2008-02-01 2009-08-06 Mitsubishi Heavy Industries, Ltd. Système et procédé de production de matière première organique à partir de biomasse brute
WO2012012594A1 (fr) * 2010-07-21 2012-01-26 E. I. Du Pont De Nemours And Company Traitement à l'ammoniac anhydre pour un meilleur broyage de biomasse
JP2012044875A (ja) * 2010-08-24 2012-03-08 Soka Univ 植物系バイオマスの糖化用担体、糖化方法および糖化装置
WO2012128055A1 (fr) * 2011-03-22 2012-09-27 昭和電工株式会社 Procédé de prétraitement de matériaux de base pour réaction hydrolytique d'une biomasse végétale et procédé de saccharification de la biomasse végétale

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006136263A (ja) * 2004-11-12 2006-06-01 National Institute Of Advanced Industrial & Technology リグノセルロース系バイオマス処理方法
JP2006141244A (ja) * 2004-11-17 2006-06-08 National Institute Of Advanced Industrial & Technology リグノセルロースの糖化方法及びそれによって得られた糖
JP2007282597A (ja) * 2006-04-19 2007-11-01 Ihi Corp 木質バイオマスの可溶化方法
JP2008271962A (ja) * 2007-04-04 2008-11-13 National Institute Of Advanced Industrial & Technology 糖の製造方法
WO2009096061A1 (fr) * 2008-02-01 2009-08-06 Mitsubishi Heavy Industries, Ltd. Système et procédé de production de matière première organique à partir de biomasse brute
WO2012012594A1 (fr) * 2010-07-21 2012-01-26 E. I. Du Pont De Nemours And Company Traitement à l'ammoniac anhydre pour un meilleur broyage de biomasse
JP2012044875A (ja) * 2010-08-24 2012-03-08 Soka Univ 植物系バイオマスの糖化用担体、糖化方法および糖化装置
WO2012128055A1 (fr) * 2011-03-22 2012-09-27 昭和電工株式会社 Procédé de prétraitement de matériaux de base pour réaction hydrolytique d'une biomasse végétale et procédé de saccharification de la biomasse végétale

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