EP0131563B1 - Verfahren zum Aufschluss von Stärke zur Herstellung von verzuckerter Maische - Google Patents

Verfahren zum Aufschluss von Stärke zur Herstellung von verzuckerter Maische Download PDF

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Publication number
EP0131563B1
EP0131563B1 EP84890107A EP84890107A EP0131563B1 EP 0131563 B1 EP0131563 B1 EP 0131563B1 EP 84890107 A EP84890107 A EP 84890107A EP 84890107 A EP84890107 A EP 84890107A EP 0131563 B1 EP0131563 B1 EP 0131563B1
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Prior art keywords
starch
temperature
enzyme
vessel
added
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Expired
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EP84890107A
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German (de)
English (en)
French (fr)
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EP0131563A1 (de
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Schahroch Dipl.-Ing. Sarhaddar
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Vogelbusch GmbH
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Vogelbusch GmbH
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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
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/06—Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch

Definitions

  • the invention relates to a process for the digestion of starch for the production of saccharified mash, raw materials containing starch being digested and liquefied above the gelatinization temperature of the starch at atmospheric pressure and the resulting mixtures being saccharified after cooling with the addition of a saccharification enzyme.
  • starch digestion Various methods of starch digestion are currently in use. However, they often have disadvantages, in particular the starch is either not fully digested or they require a large amount of energy.
  • DE-A-2018031 describes a two-stage process in which starch is gelatinized at temperatures between 85 and 170 ° C. in the first stage (A). Up to 100 ° C this step can be carried out in the presence of a-amylase.
  • the known process primarily uses so-called “sticky starches”, ie. H. starches with a high content of amylopectin. If so-called “above-ground starches” such as corn starch are used, larger amounts of enzyme must be used, and after liquefaction, heating to 130 ° C is required.
  • a suspension of starch-containing starting products that is to say a prepared, namely initially pre-gelatinized or pre-swollen slurry, is used and additionally subjected to mechanical disruption in the shear field of a rotor-stator machine.
  • the starting products are first preheated to 80 ° C and mashed with a mixture of stillage and enzyme at a mixing temperature of 90 to 92 ° C in a mixing screw.
  • a dwell time of 0.3 to 3 hours is provided for the pre-gelation taking place there.
  • Preheating of the raw materials is necessary because otherwise the temperature in the screw would drop below the gelatinization temperature of the starch.
  • EP-A-0068043 specifies that enzyme is added to the mash from the start, the enzyme being added to the hot feed water or the stillage. This leads to a partial inactivation of the enzymes.
  • the addition of acid is not mentioned in EP-A.
  • the method according to EP-A depends on the availability of a complicated homogenizing machine, it is correspondingly complex and energy-intensive. No further breakdown of the digested starch into sugars is planned.
  • GB-A-945514 relates to the production of starch syrup with a sugar content of 40 to 45%.
  • acid treatment of the syrups is recommended as a subsequent hydrolysis step.
  • the starch is converted into dextrin by introducing a mixture of the total amount of starch and the total amount of amylase in water at a temperature above the gelatinization temperature of the starch, the mixture being at a temperature range of 40 to 60 ° C, in which the used enzyme unfolds its optimal activity, is allowed to cool.
  • the conversion to sugar is continued to the desired extent, if appropriate after adding a further amount of enzyme.
  • the third variant describes the preparation of a solution of amylase in the hot water, into which solution the starch is then introduced.
  • the GB-A shows a total residence time of the starch suspension in the hydrolysis vessel of about 30 minutes.
  • the object of the present invention is to create a process for digesting starchy grains, in which process can be carried out without pretreating the comminuted raw materials and without observing the abovementioned residence times and accordingly with considerably less energy expenditure, but still achieving complete starch digestion .
  • This object is achieved according to the invention in a method of the type defined at the outset by stirring comminuted, otherwise untreated cereals into an aqueous stock liquid which is kept at a temperature of 85 to 100 ° C., preferably 90 to 95 ° C., and is in a digestion vessel , where before the acid is stirred in or a liquefaction enzyme is added while stirring in, and the digested mixture obtained is drawn off without dwell in the digestion vessel, cooled to 60 to 65 ° C. and passed to the saccharification stage.
  • Comminuted maize can be used as the cereal.
  • starch digestion was carried out almost exclusively using various high-pressure steaming processes, using temperatures between 150 and 160 ° C and pressures of 5 to 6 bar.
  • the long-known so-called cold mashing process which is carried out without pressure at temperatures below 65 ° C, is particularly suitable for cereals with a natural amylase content, such as wheat and rye.
  • a natural amylase content such as wheat and rye.
  • it is hardly carried out anymore today - especially because of the risk of infection due to the low temperature.
  • the degree of disintegration of the starch that can be achieved is usually unsatisfactory.
  • the process according to the invention avoids side reactions which lead, inter alia, to the caramelization mentioned, which has an advantageous effect on the yield, in particular when the sugar is subsequently fermented to alcohol.
  • the expenditure on equipment for carrying out the method is very low, in many cases it can be found to be sufficient with existing, slightly modified plants.
  • Thermostable a-amylases which can expediently be used as liquefaction enzymes for the process according to the invention, are easily accessible, are available in large quantities and are commercially available at any time.
  • the pH can preferably be adjusted to 1.5 to 3.5, preferably to 1.5 to 2.5, and when using liquefying enzyme as disintegrant to a value from 4.0 to 8, 0, preferably 6.0 to 7.0.
  • the comminuted cereals are expediently added within 5 to 20 minutes, preferably within 10 to 15 minutes.
  • At least some of the stillage from the distillative work-up of the saccharified mash subjected to alcoholic fermentation - optionally after separation of solids - is used as cooling liquid without cooling. Since the stillage is obtained at a high temperature anyway, this saves a large part of the heat that is otherwise required to heat up the supply liquid.
  • the digestion and the saccharification stage are carried out continuously, the crushed cereals and the stock liquid kept at a temperature of 85 to 100 ° C. being continuously fed separately to the digestion vessel and the digestion mixture continuously withdrawn from the digestion vessel and cooled and is sent to the saccharification stage.
  • the cereals are crushed in a mill 1 and temporarily stored in a storage container 2. From this container 2, the chopped cereals reach the digestion vessel 4 via a dosing screw 3, which is equipped with a stirring element 5 and a feed line 6 for enzyme solution and is connected via a line 7 to a mixing vessel 8.
  • water from supply line 9 or recirculated stillage from line 10 is prepared by admixing Ca 2 + ions from line 11, lye from line 12 or acid from line 13 or adjusted to the desired pH.
  • the aqueous feed liquid obtained in this way is brought to the desired process temperature, if necessary, by introducing live steam from line 14 and drawn off into the digestion vessel 4 via line 7.
  • Another steam supply line 15 for keeping the temperature constant during the digestion process leads to the digestion vessel 4.
  • the digested mixture is pumped into a saccharification tank 19 by opening a shut-off device 16 from the outlet on the conical bottom of the vessel 4 by means of a pump 17 via a first heat exchanger 18.
  • water intended for the supply liquid can be preheated and introduced into the mixing vessel 8 via the feed line 9.
  • Feeds for enzyme 6 ', for acid 12' and for alkali 13 'in the case of acid digestion again lead into the saccharification tank.
  • a stirring element 5 ' is also provided in the tank.
  • the saccharified mash is conveyed from the tank 19 by means of a second pump 20 via a second heat exchanger 21 after setting the desired mash concentration with water or stillage to a fermentation station (not shown).
  • a settling device 22 e.g. decanter
  • Example 1 2500 to 30001 water or decanted stillage with a temperature between 90 and 95 ° C are presented.
  • This aqueous receiving liquid is previously adjusted in the mixing vessel 8 by adding base (OH 6- ions) to a pH between 6 and 7 and mixed with Ca 2 ⁇ ions up to a content of 50 to 70 ppm.
  • base OH 6- ions
  • Ca 2 ⁇ ions up to a content of 50 to 70 ppm.
  • 1 t of ground maize is stirred in over the course of about 10 minutes, the digestion mixture being kept between the specified temperature limits by introducing live steam from line 15. After stirring in about 20 to 30% of the total amount of ground maize, thermostable a-amylase is added.
  • the digested mixture is passed into the saccharification tank 19 while flowing through the first heat exchanger 18, the mixture cooling to about 60 ° C.
  • the pH of the mixture now in the saccharification tank is adjusted to 4.5 to 5.0 by adding acid and then amyloglucosidase is added.
  • the partially saccharified mash is conveyed to the fermentation station, where it cools down to about 30 ° C. in the second heat exchanger 21.
  • the saccharified mash is then mixed with yeast mash in the fermentation tank.
  • the cooling water preheated in the heat exchangers 18 and 21 from an initial temperature of approx. 15 ° C to approx. 80 ° C is either fed directly to the mixing vessel 8 for the production of the original liquid or - if mainly decanted stillage is used as the original liquid after processing - as process water in the company or used for space heating.
  • Example 2 The procedure is analogous to Example 1, but the aqueous initial liquid in the mixing vessel 8 is adjusted to a pH between 1.5 and 2.5 by adding acid and heated to 95 ° C. by means of hot steam. No enzyme is added in the digestion vessel. The pH value in the saccharification tank is adjusted by adding lye.
  • Example 3 Continuous implementation of the method according to the invention:
  • Ground corn was adjusted from the reservoir 2 through the screw feeder 3 simultaneously with hot quench fluid, which has been previously heated in the mixing vessel 8 to 90 to 95 ° C with base (OH e- ion) to pH 6 to 7 and about 50 to 70 Contains ppm Ca 2 ⁇ ions, in a ratio of 1 part of corn meal to about 2.5 to 3 parts of feed liquid into the digestion vessel 4.
  • the predetermined amount of thermostable a-amylase is continuously metered into the digestion vessel.
  • the digestion mixture is kept at 90 to 95 ° C. with constant stirring by supplying fresh steam and, at the same time, is drawn off via the outlet at the bottom of the vessel.
  • the mash cooled to about 60 ° C.
  • the saccharification tank 19 is added to the top of the saccharification tank 19 simultaneously with the amount of acid required to adjust the pH of the mixture to 4.5 to 5.0 and with the saccharification enzyme (amyloglucosidase).
  • a dwell time of at least 30 minutes is provided for the partial saccharification of the mash.
  • the partially sweetened mash is continuously drawn off, cooled to approx. 30 ° C and, after setting the desired mash concentration with water or stillage, passed on to the fermentation station for the purpose of continuous fermentation.
  • the use of water preheated in the heat exchangers and of decanted stillage is carried out as in the batch process described in Examples 1 and 2.
  • Example 4 The procedure is as in Example 3, with the difference that the initial liquid is adjusted to a pH between 1.5 and 2.5 and no enzyme is added to the contents of the digestion container. Instead of acid is continuously fed to the saccharification liquor (OH e- ion) to adjust to a pH of 4.5 to 5.0.
  • Semi-continuous process control is also possible according to the invention if, for example, two digestion vessels are provided instead of one vessel 4 according to the drawing. While the digestion is taking place in the first vessel, material that has already been digested can be withdrawn from the second vessel.
  • the following table summarizes the results of comparative tests, based on 1 t, of starch in comminuted maize kernels (grain size less than 0.8 mm).
  • the amount of alcohol obtained in the individual experiments from 1 t starch and the amounts of NaOH, conc. H 2 S0 4 , a-amylase and amyloglucosidase (AMG) are given.
  • the dextrose equivalent and the degree of saccharification DE - ie the amount of fermentable monosaccharides present in the saccharified mash, based on the amount of anhydroglucose units theoretically present in the starch used - are also given in each case.
  • the a-amylase was used as an aqueous solution with 210,000 MWU / ml (modified Wohlgemut units), the AMG as an aqueous solution with 150 GAU / mi (glucosidase activity units).

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
EP84890107A 1983-06-09 1984-06-04 Verfahren zum Aufschluss von Stärke zur Herstellung von verzuckerter Maische Expired EP0131563B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0210883A AT387790B (de) 1983-06-09 1983-06-09 Verfahren zum aufschluss von staerke zur herstellung von verzuckerter maische
AT2108/83 1983-06-09

Publications (2)

Publication Number Publication Date
EP0131563A1 EP0131563A1 (de) 1985-01-16
EP0131563B1 true EP0131563B1 (de) 1987-08-26

Family

ID=3527936

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84890107A Expired EP0131563B1 (de) 1983-06-09 1984-06-04 Verfahren zum Aufschluss von Stärke zur Herstellung von verzuckerter Maische

Country Status (6)

Country Link
US (1) US5114491A (da)
EP (1) EP0131563B1 (da)
AT (1) AT387790B (da)
AU (1) AU563394B2 (da)
DE (1) DE3465608D1 (da)
DK (1) DK174142B1 (da)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2182936A (en) * 1985-10-12 1987-05-28 Biocon Method of producing a sugar syrup from sorghum
DE3720864C1 (de) * 1987-06-24 1988-07-28 Hrch Huppmann Maschf Gmbh Verfahren zum zusaetzlichen Aufschluss von Malzinhaltsstoffen bei Maischen fuer die Biererzeugung
US5231017A (en) * 1991-05-17 1993-07-27 Solvay Enzymes, Inc. Process for producing ethanol
US5762991A (en) * 1992-12-31 1998-06-09 Metalgesellschaft Aktiengesellschaft Continous process of producing beer
WO1996036723A1 (fr) * 1995-05-17 1996-11-21 Doru Silion Procede et installation de fabrication simultanee de l'alcool et de fourrages riches en proteines
BRPI0812042A2 (pt) 2007-06-01 2014-10-14 Sapphire Energy Uso de organismos geneticamente modificados para gerar enzimas de degradação de biomassa
BR112012032999B1 (pt) 2010-06-26 2022-11-29 Virdia, Llc Hidrolisado lignocelulósico e métodos de hidrólise ácida e desacidificação para gerar misturas de açúcar a partir de lignocelulose
IL206678A0 (en) 2010-06-28 2010-12-30 Hcl Cleantech Ltd A method for the production of fermentable sugars
IL207945A0 (en) 2010-09-02 2010-12-30 Robert Jansen Method for the production of carbohydrates
US9512495B2 (en) 2011-04-07 2016-12-06 Virdia, Inc. Lignocellulose conversion processes and products
US9617608B2 (en) 2011-10-10 2017-04-11 Virdia, Inc. Sugar compositions
CA3060976C (en) 2012-05-03 2022-08-23 Virdia, Inc. Methods for treating lignocellulosic materials
CN112226466A (zh) 2015-01-07 2021-01-15 威尔迪亚公司 萃取和转化半纤维素糖的方法
US11091815B2 (en) 2015-05-27 2021-08-17 Virdia, Llc Integrated methods for treating lignocellulosic material
CN110172402A (zh) * 2019-05-30 2019-08-27 广东中科天元新能源科技有限公司 一种淀粉质原料液糖化节能装置和工艺

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT101450B (de) * 1923-05-09 1925-10-26 Dextrin Automat Ges M B H Dext Verfahren zur Verflüssigung und Verzuckerung von Stärke.
US2989425A (en) * 1957-10-30 1961-06-20 Separator Ab Method for hydrolysis of starch
NL255881A (da) * 1959-10-02
NL261906A (da) * 1960-03-03
AU433489B2 (en) * 1968-08-14 1973-03-08 Starch hydrolysis
JPS5146817B1 (da) * 1969-04-15 1976-12-11
DE1940154A1 (de) * 1969-08-07 1971-02-25 Joseph Wall Fa Verfahren und Vorrichtung zum Aufschliessen zerkleinerter Stoffe zu Brennereizwecken
BE787674A (fr) * 1971-08-17 1973-02-19 Roquette Freres Moyens pour la liquefaction des amidons
DE2944483C2 (de) * 1979-11-03 1984-05-30 Supraton F.J. Zucker GmbH, 4040 Neuss Verfahren zur kontinuierlichen Herstellung von Alkohol aus Stärke oder stärkehaltigen Rohstoffen
US4287304A (en) * 1980-01-14 1981-09-01 National Distillers And Chemical Corp. Fermentable sugar from the hydrolysis of starch derived from dry milled corn
DE3023874A1 (de) * 1980-06-26 1982-01-21 Supraton F.J. Zucker GmbH, 4040 Neuss Verfahren zum gewinnen einer konzentrierten schlempe bei der herstellung von alkohol aus staerke oder staerkehaltigen rohstoffen
DE3125566A1 (de) * 1981-06-30 1983-01-20 Supraton F.J. Zucker GmbH, 4040 Neuss Verfahren zum kontinuierlichen mahlen und mischen von staerkehaltigen rohstoffen
US4699670A (en) * 1982-09-17 1987-10-13 Grain Processing Corporation Low D.E. starch hydrolyzates

Also Published As

Publication number Publication date
AU2895684A (en) 1984-12-13
DK283184A (da) 1984-12-10
DK283184D0 (da) 1984-06-08
ATA210883A (de) 1985-02-15
EP0131563A1 (de) 1985-01-16
AT387790B (de) 1989-03-10
AU563394B2 (en) 1987-07-09
US5114491A (en) 1992-05-19
DE3465608D1 (en) 1987-10-01
DK174142B1 (da) 2002-07-15

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