EP0256899A1 - Verfahren für die Verflüssigung von Zuckerrüben und Zichorienwurzeln durch enzymatische Hydrolyse und das so erhaltene Hydrolysat - Google Patents

Verfahren für die Verflüssigung von Zuckerrüben und Zichorienwurzeln durch enzymatische Hydrolyse und das so erhaltene Hydrolysat Download PDF

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Publication number
EP0256899A1
EP0256899A1 EP87401590A EP87401590A EP0256899A1 EP 0256899 A1 EP0256899 A1 EP 0256899A1 EP 87401590 A EP87401590 A EP 87401590A EP 87401590 A EP87401590 A EP 87401590A EP 0256899 A1 EP0256899 A1 EP 0256899A1
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EP
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Prior art keywords
enzymes
beets
hydrolysis
product
mixture
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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.)
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EP87401590A
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English (en)
French (fr)
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EP0256899B1 (de
Inventor
Régis Jacques Marie P de Baynast de Septfontaines
François Emmanuel Marie Etienne Brouard
Jean-Luc Alain Guy Baret
Yvon George Adrien Joseph Marie Gicquiaux
Hans Sejr Olsen
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.)
Socete Anonyme Dite Agro Industrie Recherches Et
Novo Nordisk AS
Original Assignee
Sucre Rech & Developpement
Novo Nordisk AS
Novo Industri AS
Socete Anonyme Dite Agro Industrie Recherches Et Developpements
Sucre Rech & Dev
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Application filed by Sucre Rech & Developpement, Novo Nordisk AS, Novo Industri AS, Socete Anonyme Dite Agro Industrie Recherches Et Developpements, Sucre Rech & Dev filed Critical Sucre Rech & Developpement
Priority to AT87401590T priority Critical patent/ATE83011T1/de
Publication of EP0256899A1 publication Critical patent/EP0256899A1/de
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Publication of EP0256899B1 publication Critical patent/EP0256899B1/de
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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
    • C13K11/00—Fructose
    • 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

Definitions

  • the invention relates to a process for the liquefaction of beets and chicory roots by the enzymatic route and the liquid hydrolyzate obtained.
  • the usual method of processing sugar beets is to cut them into thin strips (dumplings and extract the sucrose from them by diffusion. This gives a sweet juice which can be used to produce sugar for food. This sweet juice can also undergo alcoholic fermentation to produce ethyl alcohol. After extraction by diffusion, there remains a pulp which can be used, after drying, to feed livestock.
  • the present invention relates to a new process aimed at directly converting beets enzymatically into a liquid hydrolyzate, without resorting to diffusion extraction, and without the need for adding water before or during the treatment.
  • the process of the invention is applicable both to sugar beets and to fodder beets and to the hydrides of these types of beets.
  • Coarse grinding a) of beets or chicory roots can be carried out without the addition of water in any suitable type of grinder-kneader, for example of the rotary propeller type. In this stage the beets or chicory roots are crushed into small pieces of a size of the order of about 1cm.
  • the acid added in step b) can be a mineral or organic acid. Sulfuric acid is particularly suitable. The acid is added so that the pH is in the range of 3-5.5, preferably 3.5-5.
  • the mixture of enzymes used for both the prehydrolysis c) and the hydrolysis e) must comprise at least one SPS-ase, a cellulase and a cellobiase.
  • bacteriostatic agent which does not affect the action of the enzymes in step b).
  • An example of a bacteriostatic agent which can be used is formalin at the rate of approximately 0.5 to 2 liters per tonne of beets or chicory roots (0.05 to 0.2%), preferably at the rate of approximately 1 liter. per tonne (0.1%). This agent is used to prevent microbial overgrowth.
  • Bacteriostatic agents other than formalin could of course be used, but formaldehyde has the advantage of being inexpensive and readily available.
  • SPS-ase and its preparation are described in detail in FR-A-2 518 570 in the name of NOVO INDUSTRI A / S.
  • This enzyme is usually obtained from microorganisms of the genus Aspergillus .
  • SP 249 is a brown liquid with the following main specifications: polygalacturonase (EC 3.2.1.15) 9640 PGU / g pectinase 2152 KPU / g SPS-ase 29 SPSU / g cellulase (EC 3.2.1.4.) 673 A-NCU / g fungal ⁇ -glucanase (EC 3.2.1.4) 84 FBGUg hemicellulase (EC 3.2.1.78) 225 KVHCU / g
  • cellulase and cellobiase activities of SP 249 are quite low, they can be enhanced by adding additional cellulase and cellobiase enzymes. Such an addition is necessary in the case of beet processing and only optional in the case of chicory root treatment.
  • cellulase As cellulase, it is possible, for example, to use that produced by submerged fermentation of a strain of Trichoderma reesei .
  • An example of such a cellulase is the Celluclast ® product sold by the Danish Company NOVO INDUSTRI A / S.
  • Celluclast ® has a cellulase activity of 1500 ANCU / g and also has cellobiohydrolase (EC 3.2.1.91) and exo-beta-1,4D-glucosidase (EC 3.2.1.74) exo-activities and endo-endo-activity. beta-1,4D-glucanase (EC 3.2.1.4).
  • Another useful commercial cellulase is "SP-300" also from NOVO INDUSTRI A / S.
  • As cellobiase one can, for example, use that produced by submerged fermentation of a strain of Aspergillus niger .
  • An example of a cellobiase of this type is the product "Novozym 188" sold by the Danish company NOVA INDUSTRI A / S, which has a cellobiase activity of 250 CBU / g.
  • enzymes can be used in various relative proportions. As an indication, 50-75% of SP 249, 5-50% of Celluclast and 5-50% of Novozym 188 can be used, these proportions being by weight relative to the total weight of enzymes. Other enzymes such as pectinases, glucanases, galactomannases, proteases, etc. may be present in the abovementioned mixture of enzymes, if desired.
  • enzymes compared to beets or chicory roots can also vary widely. In terms of activity units per kg of dry matter contained in beets or chicory roots, enzymes can be used in the following ranges:
  • the optional enzymes may, for their part, be present in the following activity ranges:
  • activity units of the enzymes indicated correspond to the units determined by the methods developed by the company NOVO INDUSTRI A / S, which are available from this company on request.
  • the temperature during the prehydrolysis and hydrolysis stages will be between 35 and 60 ° C.
  • the temperature will be between 35 and 55 ° C during the prehydrolysis c) and between 45 and 55 ° C during the hydrolysis e).
  • the duration of the prehydrolysis stage c) can range from 1 to 6 hours, preferably 1 to 3 hours, and that of the hydrolysis e) can range from 20 to 120 hours, preferably from 24 to 72 hours.
  • Stage d) of fine grinding in the state of a slurry can be carried out in any apparatus exerting a significant shearing effect.
  • An example of a device which has been found to be particularly suitable is a deflector of the type used in the pulp industry.
  • the beet pieces are reduced to a size of the order of about 0.1 mm or less.
  • This process can be improved by combining it with one or more of the following optional improvements:
  • a first improvement consists in carrying out, before or during the coarse grinding step (a), a heat treatment of the beets or chicory roots consisting of heating them to a temperature of 70 to 90 ° C. for a few minutes an hour or so, for example using steam.
  • This heat treatment has several advantageous effects: - it facilitates the chopping of beets or chicory roots in step (a), - it makes it possible to reduce the amount of bacteriostatic agent to be used, or even to eliminate it.
  • step (a) it eliminates or greatly reduces the foaming that can occur in step (a), - it makes it possible to considerably limit the browning of the beet pieces and to obtain very slightly colored beet hydrolyzate syrups, while the products obtained without heat treatment are dark brown to black, - for a given dose of enzymes, it improves the characteristics of the hydrolyzate (lower viscosity and higher conversion rate) or allows the use of a lower dose of enzymes to obtain a viscosity and a conversion rate given for the hydrolyzate.
  • a second improvement consists in operating after the hydrolysis step (e) a post-hydrolysis carried out at an equal temperature higher than the actual hydrolysis step, preferably in the range of 55 and 75 ° C.
  • This post-hydrolysis will also usually be carried out at a lower pH than the hydrolysis, in the case where no additional enzymes are added as defined below with respect to the third improvement, while not falling below d 'a pH of 3.
  • the hydrolysis (e) is carried out at pH 4
  • the post-hydrolysis can be carried out at pH 3.
  • the pH will be adjusted according to the Optimal pH for enzymatic activity.
  • the duration of this post-hydrolysis can range from a few minutes to about 10 hours.
  • a third improvement consists in using, in addition to the mixture of enzymes defined, an invertase or an inulinase or, preferably, a mixture of these two enzymes. Addition of the enzyme or mixture of enzymes can be carried out at the rate of 100 to 10,000 INU / kg of dry matter. This addition can be carried out simultaneously with that of the other enzymes or subsequently, for example during the hydrolysis or post-hydrolysis step.
  • a mixture of fungal invertase / inulinase enzymes which is particularly suitable is that marketed under the trade name "Novozym 230" by the company NOVO INDUSTRI A / S, or a yeast invertase.
  • the invention also relates, as a new product, to an aqueous liquid product obtained directly by enzymatic hydrolysis of beets or chicory roots, characterized in that it contains, as main ingredients, glucose, fructose, polysaccharides having degrees of polymerization of 2 and 3, and nitrogen compounds, this product having an acidic pH, a viscosity not exceeding 300 mPa.s, and a content of suspended solids not exceeding 2% by weight.
  • It relates, in particular to such a liquid aqueous product having a pH of 4 to 5 and a viscosity of not more than 150 mPa.s.
  • a liquid hydrolyzed product can typically be obtained having the following characteristics: pH 4-4.5 DENSITY 1.09 VISCOSITY (mPa.s) 50-150 MATERIAL SUSPENSION 0.8-1.5 (% w / w) DRY MATERIALS REFRACTOMETRICS 20-22g / 100g solution TOTAL DRY MATERIAL (%) 24-25 TOTAL SUGARS (expressed in glucose equivalent): 160-200g / l
  • This product can be clarified to remove insoluble matter in suspension, for example by filtration or even by centrifugation, and / or concentrated, for example using a rotary evaporator.
  • the characteristics of clarified, concentrated clarified and concentrated hydrolyzates obtained from the sugar beet hydrolyzate given below are given by way of indication. above.
  • hydrolysates of the invention are useful products, in particular for the production of ethyl alcohol by conventional alcoholic fermentation using yeasts. Alcohol can be obtained with improved yields (3 to 12 percentage points more) compared to the conventional technique. Care must be taken, however, that the residual activity of the bacteriostatic agent does not hinder the development of yeasts or their fermentation activity.
  • This equipment comprises a grinder-mixer 1 of the rotary propeller type open at its upper part for the introduction of beets and the various ingredients to be incorporated (acid, bacteriostatic, enzymes), and connected to its lower part, by a conduit 2 provided from a valve 3, to a pump 4.
  • This pump 4 is itself connected to a deflector 5 by a conduit 6 provided with a valve 7.
  • the conduit 6 is connected at its middle part to a conduit 8 returning to the top of the shredder 1.
  • a conduit 9 connected to the conduit 8.
  • a valve 10 Between the connection point of the conduits 8 and 9 and the conduit 6 is provided, on the conduit 8, a valve 10, while a valve 11 is arranged on the pipe 8 just before the top of the mill 1.
  • the pipe 8 Upstream of the valve 11, the pipe 8 is connected to a pipe 12 leading to the reactor 13 with agitating blades 14, a valve 15 being provided on the pipe 12
  • An outlet pipe 16 is provided at the base of the reactor 13 and controls ée by a valve 17.
  • a jacket 18 with water circulation is provided around the reactor to adjust the temperature of the reactor, cold water or hot water can be admitted, depending on whether it is desired to cool or reheat the reactor.
  • valve 3 When the reduction in the size of the beet pieces and the degree of progress of the prehydrolysis are sufficiently advanced to make the mixture pumpable, the valve 3 is opened and the pump 4 and the shovel 5, the valves 7 and 11 being open and the valves 10 and 15 closed, so as to pass the pieces of beets through the shovel 5 and to recycle them in the crusher 1.
  • the pieces of beets see their size greatly reduced, for example at a thickness of the order of about 0.1 mm or less.
  • the valves 7 and 11 are closed and the valves 10 and 15 are opened, so as to send the beets crushed in the state of pulp or suspension and prehydrolysed, to the reactor 14 where they are left for the time necessary to complete hydrolysis.
  • the liquefied and hydrolyzed beets are evacuated from the reactor by outlet 16, after opening the valve 17.
  • the efficiency of hydrolysis is measured in these tests by the conversion rate (or liquefaction rate) X of the normally insoluble materials of beets: where So is the initial concentration of insoluble beet and St is the concentration of insoluble material at time t.
  • sugar beets were milled in a propeller mill of the LAMORT brand, of a type used in the pulp industry (pulper) in the presence of sulfuric acid additives (adjusting agent). pH), formalin (bacteriostatic agent) and mixture of enzymes.
  • the beets were treated in the grinder-mixer for approximately 1 hour by operating the latter intermittently so as not to exceed approximately 50 ° C., and subjected to three successive passes in the de-stacker, also of LAMORT brand and a type used in the pulp industry (refiner) with recycling in the mill so that the prehydrolysis time in the mill is about 2-3 hours. Then, the prehydrolized ground product was transferred to the reactor to complete the hydrolysis.
  • the proportion of formalin was 0.1% by weight relative to the weight of beets.
  • the pH and the proportion of enzymes were as indicated in the following summary table which summarizes the operating conditions of the treatment and the result of the tests.
  • This example illustrates the optional use of heat treatment.
  • the beets thus treated are then loaded into a LAMORT 201 pulper and cooled during pulping to 45 ° C, the pH is adjusted to 5 with sulfuric acid and formalin (1 liter / t) and a mixture of enzymes consisting, by weight, of 50% of SP 311, 20% of Celluclast and 30% of Novozym 188 at a dose of 11 / t.
  • SP 311 is a crude preparation of SPS-ase marketed by NOVO INDUSTRI A / S.
  • the prehydrolysis is carried out for approximately 3 hours 30 minutes, at the end of which the viscosity has decreased to 1100 mPa.s.
  • the product is then refined by two consecutive passages in a laboratory refiner (Megatron MT) 48/2).
  • the viscosity is no more than 28 mPa.s and the conversion rate of the insolubles is 78%. After 48 hours the viscosity is very much less than 30 mPa.s (measurement limit of the instrument) and the conversion rate reaches 89%.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
EP87401590A 1986-07-07 1987-07-07 Verfahren für die Verflüssigung von Zuckerrüben und Zichorienwurzeln durch enzymatische Hydrolyse und das so erhaltene Hydrolysat Expired - Lifetime EP0256899B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87401590T ATE83011T1 (de) 1986-07-07 1987-07-07 Verfahren fuer die verfluessigung von zuckerrueben und zichorienwurzeln durch enzymatische hydrolyse und das so erhaltene hydrolysat.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8609841 1986-07-07
FR8609841A FR2601036B1 (fr) 1986-07-07 1986-07-07 Procede de liquefaction de betteraves par hydrolyse enzymatique et hydrolysat liquide obtenu

Publications (2)

Publication Number Publication Date
EP0256899A1 true EP0256899A1 (de) 1988-02-24
EP0256899B1 EP0256899B1 (de) 1992-12-02

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ID=9337145

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EP87401590A Expired - Lifetime EP0256899B1 (de) 1986-07-07 1987-07-07 Verfahren für die Verflüssigung von Zuckerrüben und Zichorienwurzeln durch enzymatische Hydrolyse und das so erhaltene Hydrolysat

Country Status (10)

Country Link
US (1) US4886672A (de)
EP (1) EP0256899B1 (de)
AT (1) ATE83011T1 (de)
CA (1) CA1331357C (de)
DE (1) DE3782884T2 (de)
DK (1) DK63988D0 (de)
ES (1) ES2038193T3 (de)
FR (1) FR2601036B1 (de)
GR (1) GR3006584T3 (de)
WO (1) WO1988000243A1 (de)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2637294B1 (fr) * 1988-10-05 1991-10-18 Sucre Rech & Dev Procede et installation de production de jus sucre a partir de vegetaux amylaces
DK14292D0 (da) * 1992-02-06 1992-02-06 Novo Nordisk As Fremgangsmaade til behandling af kartoffelpulp
EP1164184B1 (de) * 2000-06-09 2005-01-05 Danstar Ferment AG Enzymmischungen enthaltend ein Enzym mit Beta-Glucanaseaktivität, ihre Verwendung zur Verminderung oder Vermeidung von Gushing
EP1162259A1 (de) * 2000-06-09 2001-12-12 Danstar Ferment AG Enzymmischungen enthaltend ein Enzym mit Beta-Glucanaseaktivität, ihre Verwendung zur Verminderung oder Vermeidung von Gushing
KR100414389B1 (ko) * 2000-10-31 2004-01-07 윤종원 치커리올리고당을 함유하는 기능성음료 및 그 제조방법
US20050100635A1 (en) * 2003-10-01 2005-05-12 Firary Mark F. Process for enzymatic treatment and filtration of a plant and products obtainable thereby
EP2256208A1 (de) 2009-05-25 2010-12-01 Süd-Chemie Ag Verflüssigte Biomasse
US8894771B2 (en) 2011-12-30 2014-11-25 Renmatix, Inc. Compositions comprising C5 and C6 monosaccharides
US20160122278A1 (en) * 2013-05-22 2016-05-05 Segetis, Inc. Process to prepare levulinic acid
DK2886648T3 (en) 2013-12-23 2018-07-02 Clariant Int Ltd Enzyme composition for hydrolysis of biomass
TWI631215B (zh) * 2017-04-25 2018-08-01 財團法人食品工業發展研究所 果寡糖組成物及其製備方法
WO2023170340A1 (en) * 2022-03-10 2023-09-14 Teknologian Tutkimuskeskus Vtt Oy Method of producing antimicrobial extract from chicory

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982000662A1 (en) * 1980-08-27 1982-03-04 A Pellegrini Process for obtaining carbohydrates from vegetal material and industrial uses for said carbohydrates

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982000662A1 (en) * 1980-08-27 1982-03-04 A Pellegrini Process for obtaining carbohydrates from vegetal material and industrial uses for said carbohydrates

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 104, no. 26, 30 juin 1986, page 169, résumé no. 227697x, Columbus, Ohio, US; G. BELDMAN et al.: "Enzymic liquefaction and saccharification of agricultural biomass", & COMM. EUR. COMMUNITIES, (REP.) EUR 1985, EUR 9940, 41pp *
ENZYME MICROB. TECHNOL., vol. 6, novembre 1984, pages 503-507, Butterworth & Co. Ltd; G. BELDMAN et al.: "Application of cellulase and pectinase from furgal origin for the liquefaction and saccharification of biomass" *
RESEARCH DISCLOSURE, no. 217, mai 1982, pages 190-193, Havant, Hampshire, GB; H.S. OLSEN: "Method for decomposition of polysaccharides, preferably plant cell wall polysaccharides, by means of a carbohydrase" *

Also Published As

Publication number Publication date
US4886672A (en) 1989-12-12
ATE83011T1 (de) 1992-12-15
DE3782884D1 (de) 1993-01-14
CA1331357C (fr) 1994-08-09
EP0256899B1 (de) 1992-12-02
GR3006584T3 (de) 1993-06-30
WO1988000243A1 (fr) 1988-01-14
ES2038193T3 (es) 1993-07-16
FR2601036B1 (fr) 1990-01-19
DE3782884T2 (de) 1993-04-08
DK63988A (da) 1988-02-08
DK63988D0 (da) 1988-02-08
FR2601036A1 (fr) 1988-01-08

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