WO2023012841A1 - Process for treating of brewing industry by-products. - Google Patents

Process for treating of brewing industry by-products. Download PDF

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Publication number
WO2023012841A1
WO2023012841A1 PCT/IT2022/050214 IT2022050214W WO2023012841A1 WO 2023012841 A1 WO2023012841 A1 WO 2023012841A1 IT 2022050214 W IT2022050214 W IT 2022050214W WO 2023012841 A1 WO2023012841 A1 WO 2023012841A1
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WO
WIPO (PCT)
Prior art keywords
lignin
hemicellulose
fraction
inorganic base
brewer
Prior art date
Application number
PCT/IT2022/050214
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English (en)
French (fr)
Inventor
Ombretta MARCONI
Assunta MARROCCHI
Original Assignee
Università degli Studi di Perugia
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.)
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Publication of WO2023012841A1 publication Critical patent/WO2023012841A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/001—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste materials, e.g. kitchen waste
    • A23J1/005—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste materials, e.g. kitchen waste from vegetable waste materials
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/12—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from cereals, wheat, bran, or molasses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B01D11/0284—Multistage extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
    • B01D9/0054—Use of anti-solvent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G1/00—Lignin; Lignin derivatives
    • 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
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12F—RECOVERY OF BY-PRODUCTS OF FERMENTED SOLUTIONS; DENATURED ALCOHOL; PREPARATION THEREOF
    • C12F3/00—Recovery of by-products
    • C12F3/06—Recovery of by-products from beer and wine
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K10/00—Animal feeding-stuffs
    • A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
    • A23K10/37—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material
    • A23K10/38—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material from distillers' or brewers' waste
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention belongs to the technical field of food industry by-product treatment and recovery, more specifically it belongs to the field of treatment and recovery of brewing industry by-products, specifically the residual spent grains from brewing process, i.e., the mash- ing residue consisting of malt husks and other insoluble parts remaining from the mashing process.
  • Brewer' s spent grains constitute the main by-prod- uct of the brewing industry, accounting for about 85% of the total waste from the brewing process. On average, the annual production of brewer's spent grains is about 40 million tons, of which about 8 million are produced in Europe alone and 240, 000 t/year in Italy. Only 30% of brewer's spent grains are currently reused, mainly as feed in the livestock sector, while most are disposed of in landfills.
  • Cellulose is used in a variety of sectors, for example, in the production of paper and cardboard, or as an additive in polymeric materials, or even in the production of bioethanol; cellulose can also be converted into deriva- tives such as cellophane, rayon, cellulose acetate, typi- cally used in textiles, for the production of plastics, var- ious consumer products, etc.
  • Hemicellulose and lignin are typically regarded as low-quality and low-value by-products, yet they can be used as substrates in bio-refineries for the production of a very wide range of bio-products of industrial interest, such as raw materials for chemicals, additives, biofuels and even energy .
  • hemicellulose conversion processes have been developed for the production of ethanol, xylitol, butanediol, polyhydroxyalkanoates, organic acids (succinic acid, butyric acid, etc. ) , furfural (Chandel et al, Bioconversion of hemicellulose into ethanol and value-added products, 2018) ; in this case, the extraction of hemicellulose in the form of monomeric sugars is required.
  • Also known are uses of hemicellulose in macromolecule form as a source of new materials, with special reference to composite materi- als .
  • lignin Possible uses include: the use of depol- ymerized lignin in polyf unct ional aromatic monomers for use as a raw material in the polymer industry; the use in mac- romolecule form as an additive, or in polymer mixtures, or composites in the synthesis of copolymers; the use of lignin as a source of carbon-based materials such as carbon fibers.
  • lignin there is, however, a particular need to obtain high-quality lignin and hemicellulose, i.e., with a high degree of purity, which can be directly reused for other purposes in a wide variety of production sectors, without the need for further processing.
  • Patent application WO 2020/214502 Al discloses a process for extracting the spent grains from which a protein fraction and a fiber-rich fraction are isolated; separation is done using a classifier mill. The fibrous fraction is then processed into paper material for packaging; in one possible form of implementing the method, preliminary drying of the spent grains to moisture values less than or equal to 70% is provided.
  • Methods are also known for recovering the protein component and cellulose, in the form of nanofibers, by al- kaline treatment of dried brewer's spent grains; other known methods allow the recovery of hemicellulose alone in hydro- lyzed form (Mussatto et al., Chemical characterization and liberation of pentose sugars from brewer' s spent grain, Jour- nal of Chemical Technology and Biotechnology, 2006) , of cel- lulose alone (hydrolyzed and non-hydrolyzed) (Mussatto et al., Optimum operating conditions for brewer' s spent grain soda pulping, Carbohydrate Polymers, 2006; Mussatto et al., Effect of hemicellulose and lignin on enzymatic hydrolysis of cellulose from brewer' s spent grain, Enzyme and Microbial Technology, 2008) and lignin alone (Mussatto et al. , Lignin recovery from bre
  • Patent application WO 2020/234761 Al describes a process for recovering only the components of the lignocel- lulosic structure (lignin, hemicellulose, cellulose) from biomass, including brewer's spent grains.
  • This process in- volves the use of deep eutectic extraction (DES) solvents, but these are very expensive, especially in view of an in- dustrial-scale application.
  • DES deep eutectic extraction
  • the use of choline acetate in combination with glycolic acid is contemplated; disadvantageously, both gly- colic acid and the direct precursor of choline acetate, cho- line hydroxide, have toxic properties for humans and the environment.
  • the process illustrated in WO 2020/234761 Al involves preliminary drying of the spent grains, and their components are selectively isolated using additional organic solvents (ethanol) , which increases the costs associated with the process.
  • Another currently known process for recovering cellulose, hemicellulose, and lignin from brewer's spent grains involves the use of ionic liquids as the lignin ex- traction solvent (Outeirino et al., A novel approach to the biorefinery of brewery spent grain, Process Biochemistry; Biorefining brewery spent grain polysaccharides through biotuning of ionic liquids , Carbohydrate Polymers, 2019) .
  • the use of such ionic solvents entails economic disadvantages due to their high cost, all the more so in view of indus- trial-scale applications; moreover, this method is limited to obtaining only lignin in macromolecule form and cellulose and hemicellulose in hydrolyzed form.
  • Patent US 10240006 B2 discloses a method for iso- lating functionalized lignin from lignocellulosic biomass by hydrolysis under supercritical conditions combined with re- active extraction. The method, however, is limited to ob- taining only lignin in macromolecule form, and cellulose and hemicellulose in hydrolyzed form.
  • Patent application US 5430142 A relates to a pro- cess for the isolation of functionalized xylans from ligno- cellulosic biomass by reactive extraction.
  • this process involves preliminary delignification of the biomass by an organosolv process and/or treatment by hypochlorites, which can have significant negative environmental impacts.
  • fractionation refers to the subdivision of a heterogeneous product, such as indeed brewer's spent grains, into the fractions of homogeneous component elements, namely, in the present case, protein, cellulose, hemicellu- lose and lignin.
  • the object of the present invention is to provide a technique for deconstructing, separating, and integrally recovering the components of brewer's spent grains, thus enhancing the value of these waste by-products, making it possible to reuse them in other processes, and reintroducing them into a production cycle.
  • a second object of the present invention is to provide a process for recovering the components of brewer' s spent grains that does not require prior dewatering, drying, or desiccation of the wet spent grains resulting from the brewing process, so as to reduce costs, both from an energy and economic point of view.
  • Further object of the present invention is to pro- vide a process for the fractionation of the essential com- ponents constituting the brewer's spent grains, also func- tionalized, with a high degree of purity.
  • Not least object of the present invention is to provide a process for the separation of the protein component of brewer' s spent grains and for the separation of the lig- nocellulosic component into cellulose, functionalized hemi- cellulose, and lignin, possibly functionalized.
  • the present invention comprises a reactive extraction step i.e., with simultaneous function- alization and extraction (by precipitation) of hemicellu- lose, thus enabling hemicellulose to be obtained in the form of a high-quality (pure) and functionalized macromolecule, increasing its value for biorefineries.
  • the process includes a combination of the functionalization and extrac- tion by precipitation of lignin, for example, by means of alkyl-type organic compounds (preferably hydroxyalkyls) .
  • the treatment process object of the present invention can be implemented semi-continu- ously or continuously, so as to improve efficiency and ensure absolute benefits from the point of view of the safety of operators .
  • fractions that are isolated by means of the present process exhibit a high degree of purity, being basically composed of a homogeneous component (protein, cellulose, hemicellulose or lignin) without a significant presence of other foreign elements.
  • Fig. 1 shows a flow chart of a form of implemen- tation of the process for treating brewer' s spent grains according to the present invention.
  • Entering step (A) are the spent grains (1) , water and an inorganic base (NaOH) , and exiting this step are the proteins (2) and fibers (3) , which then enter step (B) where they are combined with water and an inorganic base (NaOH) , following this step, cellulose (4) , and hemicellulose (5) and lignin (6) are obtained solubilized.
  • Hemicellulose (5) and lignin (6) supply step (C) where an organic compound is added that selectively reacts with hemicellulose (5) , and further downstream, functionalized hemicellulose (7) and solubilized lignin (6) are obtained, the latter feeds step (D) , together with a strong acid (11) and produces a solid fraction containing lignin (8) , finally obtaining water and salts (9) .
  • step (D) functionalized lignin can be obtained if an organic compound is substituted in place of the strong acid.
  • the present pro- cess of fractionation of the components of wet brewers' spent grains takes place in a single reactor and includes the following main steps :
  • step (A) wet brewer' s spent grains resulting from a brewing process are fed into a discontinuous, semi- continuous or continuous reactor operating at atmospheric pressure and are mixed with a fluid consisting of water and an inorganic base, preferably sodium hydroxide (NaOH) .
  • a fluid consisting of water and an inorganic base, preferably sodium hydroxide (NaOH) .
  • the volume of water is such that the concentration in water of the inorganic base, preferably sodium hydroxide, is between 2, 5% and 6% m/V, considering a quantity of inor- ganic base between 2, 5% and 6% by weight relative to the dry matter of the spent grains; optimum results are obtained with a quantity of inorganic base between 4, 5% and 5, 5% by weight.
  • the process temperature is maintained between 30 °C and 90°C, preferably between 50° and 70°C.
  • the mixture is maintained under intermittent or continuous stirring for be- tween 0.5 and 5 hours, preferably at least 2 hours.
  • step (A) is preceded by the grinding of wet brewer's spent grains. Grinding facili- tates the mixing of the spent grains themselves with the liquid extracting medium during step (A) and, consequently, subsequent separation processes.
  • the brewer' s spent grains treated with sodium hydroxide in an aqueous solution result in a mixture consisting essentially of a first liquid frac- tion comprising solubilized proteins, and a first solid frac- tion, the latter comprising the lignocellulosic fibrous fraction of the brewer's spent grains, which in turn consists of hemicellulose, cellulose and lignin.
  • step (A) the protein component is solubilized, generating a first liquid fraction comprising protein and a first solid fraction comprising hemicellulose, cellulose and lignin .
  • step (A) the separation between the insoluble lignocellulosic residue and the liquid portion is refined by conventional methods such as filtration or centrifugation .
  • the solid residue result- ing from the previous step (A) i.e., the fiber
  • the vol- ume of water is such that the concentration in water of the inorganic base, preferably sodium hydroxide, is between 2, 5% and 6% m/V, considering a quantity of inorganic base between 30% and 55% by weight with respect to the dry matter of the fiber.
  • the process temperature is preferably maintained be- tween 30°C and 90°C.
  • the mixture can be kept under intermittent or con- tinuous stirring for between 0.5 and 24 hours, preferably at least 6 hours .
  • step (B) the separation of the cellulosic solid residue from the liquid fraction is refined by conventional methods such as filtration or centrifuga- tion.
  • the liquid fraction is used in the next step (C) .
  • the liquid fraction from the previous step (B) is mixed inside the reactor with an organic compound.
  • the concentration of the organic compound in the liquid fraction is between 1% and 9% m/V, preferably between 4% and 6% m/V.
  • the organic compound can be any suitable organic compound that selectively reacts with hemicellulose at a process temperature below 100°C, preferably forming ester, ether, or amide bonds with it.
  • the mixture can be kept under intermittent or continuous stirring for between 0.5 and 2 hours, preferably at least 1.5 hours.
  • the resulting mixture consists essentially of a third liquid fraction containing solubilized lignin and a third solid fraction comprises functionalized hemicellulose.
  • dur- ing step (C) a reactive separation of the hemicellulose oc- curs by means of the organic compound: the hemicellulose contained in the liquid fraction is functionalized by ester- ification, etherification, and amidation, and as the reac- tion progresses, precipitation of the functionalized hemi- cellulose occurs due to the progressive decrease in the sol- ubility characteristics of the derivative.
  • the organic compound used is benzoyl chloride, which func- tionalizes hemicellulose by esterification.
  • step (C) the separation between the function- alized hemicellulose and the liquid fraction is refined by conventional methods such as filtration or centrifugation.
  • the precipitate obtained is washed with water, or ethanol, or both, to remove possible residual organic compound and other impurities.
  • the liquid fraction is used in the next step (D) .
  • step (D) of the present process the liquid fraction resulting from step (C) is acidified to pH between 2 and 3 with a strong acid such as, for example, a mineral acid such as hydrochloric acid or sulfuric acid.
  • a strong acid such as, for example, a mineral acid such as hydrochloric acid or sulfuric acid.
  • the result- ing suspension consists essentially of lignin, and the lat- ter is separated from the liquid fraction, consisting essen- tially of water and salts, by centrifugation.
  • step (C) is followed by the step (E) of extraction of functionalized lignin.
  • step (E) the liquid fraction from step (C) is additioned with an alkyl-type organic compound, preferably alkylthiols, with which it reacts to form a solid fraction comprising the functionalized lignin and the supernatant.
  • an alkyl-type organic compound preferably alkylthiols, with which it reacts to form a solid fraction comprising the functionalized lignin and the supernatant.
  • Said organic compound can be any organic compound having characteristics such that it reacts with lignin, preferably with the phenolic -OH functional groups of lignin, at a temperature below 100°C.
  • the protein content in the liquid portion result- ing from the first step (A) of the process was measured by total nitrogen determination.
  • the test was carried out according to standard AOAC 945.18-B and AOAC 920.53 methods. The operation was repeated on the fibrous residue.
  • the pro- tein separation efficiency given by the ratio: [Protein in liquid fraction (g) /total protein in liquid and fiber frac- tion (g) ]x 100, was greater than or equal to 40 %.
  • the separation efficiency of cellulose was found to be greater than 80%.
  • the yield of functionalized hemicellulose was found to be more than 85%.
  • results are reported for the reac- tive extraction of hemicellulose present in the liquid frac- tion from the second step (B) of the process using a prede- termined amount of benzoyl chloride (step C) , carried out at a temperature preferably between 30°C and 50°C for between 1 and 2 hours, in the presence of NaOH (concentration: 2, 5% to 6% m/V) .
  • the amount of lignin recovered by precip- itation with mineral acid from the liquid portion extracted in the fourth step (D) of the process was determined gravimet rically after drying at 60 °C for about 24 hours. A lignin recovery efficiency greater than 78% was measured.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Holo Graphy (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
PCT/IT2022/050214 2021-08-05 2022-07-21 Process for treating of brewing industry by-products. WO2023012841A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT102021000021299A IT202100021299A1 (it) 2021-08-05 2021-08-05 Processo di trattamento di sottoprodotti dell’industria birraria
IT102021000021299 2021-08-05

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WO2023012841A1 true WO2023012841A1 (en) 2023-02-09

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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5430142A (en) 1993-08-06 1995-07-04 The Center For Innovative Technology Thermoplastic pentosan-rich polysaccharides from biomass
AU2015252877A1 (en) 2014-05-01 2016-10-27 Renmatix, Inc. Upgrading lignin from lignin-containing residues through reactive extraction
GB2596666B (en) 2019-04-19 2023-02-22 Coors Brewing Co Packaging and products made using spent grains
CA3140607A1 (en) 2019-05-23 2020-11-26 Politecnico Di Milano Process for biomass treatment

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"Doctoral Dissertations", vol. 45, 1 January 2016 (2016-01-01), pages 1 - 125, XP055782299, Retrieved from the Internet <URL:https://www.vttresearch.com/sites/default/files/pdf/science/2016/S124.pdf> *
HE YANHONG ET AL: "Wet fractionation process to produce high protein and high fiber products from brewer's spent grain", FOOD AND BIOPRODUCTS PROCESSING, INSTITUTION OF CHEMICAL ENGINEERS, RUGBY, GB, vol. 117, 25 July 2019 (2019-07-25), pages 266 - 274, XP085805695, ISSN: 0960-3085, [retrieved on 20190725], DOI: 10.1016/J.FBP.2019.07.011 *
SOLANGE I MUSSATTO: "Brewer's spent grain: a valuable feedstock for industrial applications : Brewer's spent grain and its potential applications", JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, vol. 94, no. 7, 24 January 2014 (2014-01-24), GB, pages 1264 - 1275, XP055427382, ISSN: 0022-5142, DOI: 10.1002/jsfa.6486 *

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