US3640768A - Process for hydrolytic degradation of cellulosic materials to sugars - Google Patents

Process for hydrolytic degradation of cellulosic materials to sugars Download PDF

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US3640768A
US3640768A US767669A US3640768DA US3640768A US 3640768 A US3640768 A US 3640768A US 767669 A US767669 A US 767669A US 3640768D A US3640768D A US 3640768DA US 3640768 A US3640768 A US 3640768A
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vessel
temperature
steam
hydrolysis
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Rudolf Eickemeyer
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00—Digesters
    • 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
    • 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
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes

Definitions

  • ABSTRACT Cellulosic materials are chemically degraded in a percolator vessel by introducing a liquid agent from below into the cellulosic materials placed above the filter area of the vessel while the vessel is at about atmospheric pressure and introducing steam at a higher pressure than atmospheric from below the cellulosic material to raise the temperature in the vessel to at least 100 C., the displaced air being permitted to escape and then introducing steam at a pressure of about 1 atmosphere above atmospheric pressure from the top of the vessel to expel the liquid which is in excess of the absorptive power of the cellulosic material through the bottom of the vessel and then introducing further steam from the bottom of the vessel to bring up the temperature to the reaction temperature and recovering the reaction product.
  • the invention also embraces a vessel for practising the above process which is provided with a filter subdivided in at least two sections, one over the other, and provided with multilevel horizontal rows of perforations having a minimum diameter of 2-5 mm., increasing towards the periphery of the filter, and having a cross section of 0.2 to 4 percent of the cylindrical cross section of the percolator vessel, measured at the narrowest point of the conical holes, the rows of perforations preferably having a downwardly decreasing distance from each other.
  • the conventional processes of this type are designed in a manner that the cellulosic material is first subjected to heat by means of steam in order to dispel the air from the percolator. It has also been proposed to evacuate the percolator prior to heating in order to remove at least the major part of the air. The reaction liquid is then added subsequently to the initial heating step. The liquid is usually preheated to a temperature above 100C. Very substantial amounts of liquid are necessary to effect the impregnation of the material up to saturation because of the absorptive power of cellulosic materials.
  • the present invention therefore has the object of obtaining a uniform impregnation of the entire material in the percolator with a comparatively small amount of steam.
  • Another object of the invention is a process of this type wherein a comparatively high concentration of different desired final products, in particular sugar solutions, is obtainable.
  • Another object is to provide a process of this type wherein not only low amounts of steam may be used but where there are also limitations on the necessary amounts of reaction liquid without having an unfavorable effect on the concentration of the final reaction product.
  • a process for the chemical degradationof cellulosic materials by percolating a liquid agent therethrough comprising a. supporting the material in a closed percolator vessel at a level intermediate the top and bottom end of the vessel above the filter area ofthe vessel;
  • the invention also embraces a percolator vessel for the process described which has a filter subdivided in two sections, one over the other, and provided with multilevel horizontal rows of perforations having a minimum diameter of 2-5 mm.', increasing towards the periphery of the filter, and
  • the rows of perforations preferably having a downwardly decreasing distance from each other.
  • the invention involves as a firststep the introduction of the reaction liquid and steam at a temperature of at least whereby a reaction liquid steam mixture rises upwardly in the percolator.
  • a reaction liquid steam mixture rises upwardly in the percolator.
  • the open space between the cellulosic particles is completely taken up and in addition the reaction liquid will penetrate into the individual particles and the displaced air in each case will rise towards the top.
  • the charge may be drained downwardly through the filter. It is only after this step that the remaining material which is now just saturated with liquid is heated by the admission of steam through the filter and is thus brought up to the reaction temperature.
  • the reaction liquid will be a suitable mineral acid solution of which the ion concentration in the first stage where the saccharification of the hemicellulose is effected may amount to about that of a 1 percent concentrated sulfuric acid, while in the second stage where the cellulose is subjected to saccharification after the sugars formed from the hemicellulose have been washed out at a reduced temperature and reduced acid concentration, acid may be used of which the ion concentration is equivalent to that of a 3-5 percent sulfuric acid.
  • a preliminary hydrolysis of the hemicellulose of the pentosane-containing starting material is effected followed by an alkali conversion of the cellulose.
  • the process of the invention contemplates that in this case a reaction liquid is used for at least part of the conversion of the hemicellulose consisting of dilute mineral acid solution having a hydrogen ion concentration corresponding to about 1 percent sulfuric acid.
  • the reaction temperature should be below C. This will be followed by a washing out of the sugars formed from the hemicellulose at reduced temperature and acid concentration by means of a plurality of liquid charges of reduced sugar concentration. These charges may be obtained from previous percolation runs.
  • the lastwash is effected with water.
  • reaction liquid which contains solvents for the lignin such as sodium hydroxide, sodium sulfide and sodium carbonate in a concentration to provide for the necessary re-' agent in the cellulosic material after expulsion of the excess liquid.
  • a reaction temperature in this stage is used of at least 140 C.
  • the soluble alkali lignin is then again washed out by means of a plurality of liquid charges of decreasing temperature and decreasing concentration of alkali lignin and other unspent reagent. These liquid charges are again obtained from previous percolation runs. Finally, there follows a wash with water. The necessary temperature is accomplished by means of steam which is introduced in each case between two charges. As a result, pure cellulose will remain in the percola- I01.
  • nitric acid of a hydrogen ion concentration as indicated is used, at least in case of the hemicellulose saccharification, that is during the preliminary hydrolysis, but possibly also during the hydrolysis of the cellulose.
  • the fresh reaction liquid which is necessary for the conversion of the cellulose may contain alkali lignin obtained from a previous percolation run in addition to fresh solvents for the lignin.
  • the fresh reaction liquid consistsat least partially of one or several discharges resulting from previous lignin solution percolations to which the necessary additional fresh chemical may be added.
  • the subsequent reaction time necessary to accomplish the saccharification of the'hemicellulose or cellulose is of course'accompanied also by decomposition of the formed sugar under the conditions of the reaction.
  • a certain flattening out of the possible maximum sugar concentration occurs after a certain reaction time. The sugar concentration at a continuation of the reaction would decrease.
  • reaction time is selected so that the formed sugar has at least 70 percent, and at most 90 percent, of its possible maximum concentration. when thispoint is reached the sugar is then washed out at a reduced temperature and acid concentration. New reaction liquid is subsequently added, particularly in cases of the saccharification of the cellulose followed again by washing out at reduced temperature and acid concentration.
  • the elution or washing out of the formed sugar can be effected by a plurality of liquid charges as indicated.
  • the temperature is preferably l30l40 C. for the conversion of the hemicellulose with a reaction time of about 40 minutes.
  • the temperature is l60-'l70 C. with a reaction time of 40 minutes, and in the second stage of the conversion-of the cellulose the reaction temperature is between 170 and 190 C., preferably 180 C. reaction time of 30 minutes.
  • a suitable apparatus for operating the described process is a percolator which in its lower conical section has a vertically subdivided filter.
  • the filter comprises a plurality of filter trays held in flanges of the conical wall portions of the percolator.
  • the filter trays have perforations with a diameter which increases from the center to the periphery.
  • the minimum diameter is between 2 and millimeters, preferably between 3 and 4 millimeters
  • the perforations are distributed at about equal distances throughout the entire filter surface.
  • the total cross section of all perforations is between about 0.2 and 4 percent, preferably between 0.5 and 1.5 percent, of the inner percolator cross section measured at the narrowest point of the conical holes.
  • the two sections of the filter are sealed against each other and are provided with a number of inlets which are arranged uniformly at the periphery of the conical portion and are controlled by common control valves.
  • the filter is divided into two separate sections. It is, however, also possible to use more than two sections.
  • a further feature of the invention is the arrangement of the perforations in a manner that the perforations in the different superposed levels have a distance from the preceding level which decreases downward and at the lowermost levels is about one-half to one-third of the maximum level existing in the top levels.
  • the perforations of the several perforation trays or levels are preferably set off against each other so that the distance of the individual perforations be as uniform as possible.
  • the upper outer wall of the conical filter portion is preferably without perforations in order to prevent undesirable peripheral circulation of the steam and liquid.
  • the lower filter portion has about 50-67 percent more perforations than the upper filter portions
  • EXAMPLE 1 Thirty-three t. of beech shavings containing about 26 t. dry wood substance were placed in a percolator having a contents of 100 m. and a diameter of 3.2 m. in its upper cylindrical portion 1, while the lower conical portion 2 had an inclination of 60 and a total height of 2.7 m.
  • the percolator also was provided with a top dome 3 in which there were disposed rapidaction closures 3', a liquid valve 4 and a steam inlet valve 5, as well as a steam outlet valve 6 and a distributor 4' for both the liquid and the steam.
  • the beech shavings were then subjected to a preliminary hydrolysis to xylose and to a main hydrolysis to dextrose followed by a processing of the lignin residue.
  • the percolator consisted of copper-plated sheet steel and was adjusted to withstand an operation pressure of 13 atmospheres above atmospheric pressure.
  • a vertically subdivided filter consisting of copper sheets 7, 7' was installed which was supported by flanges 8.
  • the upper filter portion 7 had a height of about 700 mm. measured in the wall portion of the conical section of the percolator and was sealed against the lower filter portion 7' which had a height of about 1,400 mm. (measured again in the conical wall portion) by a sealing ring 9.
  • the upper filter section had perforations of conical form arranged in horizontal rows 10.
  • the perforation had a diameter at the center of about 3 mm. and at the periphery of about 5 mm. with a horizontal distance from each other of 50 mm.
  • the rows of perforations in the top levels were spaced by 50 mm. which was reduced at the lower edge of the upper filter section V to about 40 mm.
  • the perforations of the individual rows were offset against each other.
  • the lower filter section likewise had perforations l0 arranged in horizontal rows and having the same diameters and same horizontal distances. At the upper edge of the lower filter section the distance of the perforation rows was about 40 mm. which was reduced gradually up to the lower edge to about 20 mm. The perforations of the individual rows again were offset against each other.
  • percolators which are steel plated with a nickel-chromium, noncorroding steel (V 4 A) which are similar to the conventional cellulose boilers-The filter in the conical portion in this case likewise is formed from V 4 A sheet steel. This type of filter is particularly useful for obtaining pure cellulose after carrying out the preliminary hydroly- SIS.
  • the upper steam outlet valve 6 was closed and steam was admitted through the upper inlet valve 5 into the upper section of the percolator until a pressure of about 1 atmosphere above atmospheric was reached, which was then maintained at a constant value by adjusting further admission of steam.
  • the excess liquid of about 25 m. was drained through both filter sections by opening the valve 12' and by means of the control valve 13, while a pressure difference was maintained between the percolator top section and the space behind the filter (impulse control device 14) between zero at the beginning of the discharge and increasing gradually to 0.5 atmospheres at the end of the discharge, which altogether lasted for about minutes.
  • the charge which now was saturated with dilute sulfuric acid was then heated, after closing the control valve 13 and opening the valves 11 and 15, to a temperature of 135 C. by admitting steam through the two filter sections.
  • the temperature corresponded to a saturated steam pressure in the percolator upper part which resulted from maintaining a pressure difference of at least 9.8 atmospheres between the lower and the upper portion by means of the impulse control device 14.
  • the liquid was then drained through the valve 13 by adjusting the pressure difference between the upper percolator part and the space behind the filter sections to a value of initially zero, and then increasing during the reaction time of about 15 minutes to a value of 0.5 atmospheres.
  • the first discharge and part of the second discharge constituted the so-called extraction amounting to 5.9 t. extract having a xylose contents of 4.7 t. in an about 9 percent solution. This corresponded to a yield of 18 percent of the beech wood dry substance. This extract could then be processed further to the desired final products.
  • the remaining discharges were saved for making the extraction charges 1 to 4 for the next run. They were stored in storage vessels.
  • the fifth and sixth charge preferably consisted of deionized water.
  • Second Stage-Hydrolysis of Cellulose After completion of the preliminary hydrolysis, which at the end proceeded with a temperature of only slightly above 100 C., a new charge was added in an amount of 40 m. at a temperature of about and consisting of about 4 percent sulfuric acid. This charge was added from below through the upper section of the filter while at the same time steam was introduced through the lower filter section in order to obtain a mixing temperature of at least C.
  • the steam percolator pressure in the upper section was increased to 1 atmosphere above atmospheric by a heavy addition of steam from the top. This pressure was then maintained by admitting controlled additional amounts of steam. The excess liquid was again drained through the liquid outlet valve after adjusting the pressure difference to a value of zero at the beginning of the discharge and increasing to about 0.5, this pressure difierence existing between the percolator upper por-. tion and the space behind the filter. The discharge lasted. about 15 minutes.
  • a reaction temperature was then established of about C. by introducing steam through the entire filter surface at a pressure difference of at least 0.8 atmospheres between the lower and the upper section of the percolator. This reaction temperature corresponded to the 1 saturation steam pressure in the percolator upper part. The time for heating to the desired temperature amounted to about 20 minutes.
  • EXAMPLE 2 It may be of interest in a particular case only to go through the preliminary hydrolysis and subsequently to obtain the lignin from the more or less still intact cellulose of the starting material such as beechwood.
  • the preliminary hydrolysis in this example therefore was the same as in example 1 except that a shorter reaction was used in order not to damage the cellulose and also employing nitric acid instead of sulfuric acid in order to be able to work with a percolator that was plated with chromium nickel steel plates of the V 4 A type.
  • the concentration of the xylose solution is therefore rate thereby was reduced from 18 percent to betweensomewhat lower and in case of somewhat reduced amounts of liquid amounted to about 8.0 percent.
  • This step was followed by the washing out of the formed alkali-lignin by means of a plurality of liquid charges which had been obtained from the waste liquor of the previous runs.
  • the first or the first two discharges however were eliminated. These discharges contained the highest concentration.
  • the last two charges of liquid were again water in order to obtain a well-washed cellulose.
  • the temperature in the percolator could be kept at a decreasing level for consecutive extraction steps similar to the previously described operation.
  • Thetemperature prior to the last charge should still be at least 1 10 C.
  • the following table illustrates the details of the proceeding.
  • the first discharge containing 10 t. of waste liquor-dry substance was then split as follows: 3.2 t. waste liquor-dry substance and 15 t. water were used together with the excess from the reaction which contained 1 t. fresh reagents, l t. waste liquor-dry substance and 15 t. water for the purpose of dissolving 3.2 t. fresh reagents containing about 0.4 t. filler materials.
  • fresh reagents it is, of course, also possible to use the melt from the fin'ng of the liquor which then must be sub jected to an alkaline treatment. The total solution was used as a charge for the next run.
  • the mixture Prior to these reaction-extraction steps, the mixture may be heated in a similar manner as in the preceding examples to between 140 and 150 C. and be maintained at this temperature for l5 to 30 minutes.
  • the further extraction charges could be carried out at stepwise lower temperatures.
  • a cellulose (12 to 13t. of dry substances) having a high content of a cellulose which could then be evacuated with water to a cellulose storage tank and could later be submitted to further processing.
  • a process for the chemical degradation of a cellulosic material by percolating a liquid agent therethrough comprismg a. placing the said material in a closed percolator vessel having two superposed filter areas of downwardly diminishing cross section and supporting the material at a level intermediate the top and bottom end of the vessel and above the said two filter areas;
  • cellulosic material consists of wood shavings, wherein the product extracted in the preliminary hydrolysis is principally xylose, and wherein the product extracted in the hydrolysis of the cellulose is primarily dextrose.
  • reaction temperature during the preliminary hydrolysis in the first stage is l30-140 C. at a reaction time of about 40 minutes and wherein in the second stage the hydrolysis of the cellulose is effected initially at a temperature of to C. during a reaction time of about 40 minutes and thereafter at a temperature of 170 to C. during a time of 30 minutes.
  • washing out of the sugars formed in the reaction is effected with a plurality of liquid charges of decreasing sugar concentration obtained from previous runs followed as a final step by a washing with water.

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  • Biochemistry (AREA)
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US767669A 1967-10-17 1968-10-15 Process for hydrolytic degradation of cellulosic materials to sugars Expired - Lifetime US3640768A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3928121A (en) * 1973-10-23 1975-12-23 Zepeda Castillo Enrique Process for the obtention of fermentable powdered syrup and alphacellulose from xerophyte plants
US4025356A (en) * 1974-01-16 1977-05-24 Anstalt Gemass Method for continuous hydrolysis of pentose containing material and apparatus for implementing the method
US4087316A (en) * 1975-09-02 1978-05-02 Cotton Incorporated Process for obtaining seed hull commodities including cellulosic fibers and xylitol
US4138272A (en) * 1977-11-15 1979-02-06 Zepeda Castillo Enrique Process for the obtention of fructose and fructose-rich syrups from xerophyte plants
US4160695A (en) * 1976-07-20 1979-07-10 Projektierung Chemische Verfahrenstechnik Gesellschaft Mit Beschrankter Haftung Process for the production of glucose from cellulose-containing vegetable raw materials
US4664832A (en) * 1984-09-28 1987-05-12 State Of South Dakota As Represented By The Department Of Transportation Deicing chemicals and their preparation from polysaccharide sources
US4708746A (en) * 1981-12-15 1987-11-24 Werner & Pfleiderer Method the hydrolytic splitting of acid treated comminuted crude cellulose with steam

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IT1025544B (it) * 1973-11-23 1978-08-30 Sued Chemie Ag Processo per disgregare legno di latifoglie
IT1025347B (it) * 1973-11-23 1978-08-10 Sued Chemie Ag Processo per la disgregazione di gusci di avena
CH585794A5 (xx) * 1974-12-03 1977-03-15 Sulzer Ag
US3990904A (en) * 1976-05-11 1976-11-09 Sud-Chemie Ag Method for the preparation of xylose solutions
GB1548500A (en) * 1977-05-17 1979-07-18 Inst Voor Bewaring Process for obtaining xylose by hydrolysis of residues of annuals
DE3107950A1 (de) 1981-03-02 1982-09-16 Percolysis Verfahrenstechnik GmbH, 8000 München "verfahren und vorrichtung zur verzuckerung von cellulosematerialien, wie holz und holzabfaellen, sowie einjaehrigen pflanzen, wie stroh etc. durch hydrolyse mit verduennten saeuren und erhoehten temperaturen und drucken, sowie auswaschung des jeweils gebildeten zuckers unter wesentlich milderen temperatur- und druckbedingungen zur gewinnung von zuckerloesungen, die der vergaerung zu alkohol als treibstoff zugefuehrt werden, ggf. unter gewinnung von nebenprodukten"
US5023103A (en) * 1987-01-27 1991-06-11 D. D. Williamson & Co., Inc. Fiber and method of making
DE3729428A1 (de) * 1987-09-03 1989-03-16 Werner & Pfleiderer Verfahren und vorrichtung zur hydrolytischen spaltung von cellulose
US5424417A (en) * 1993-09-24 1995-06-13 Midwest Research Institute Prehydrolysis of lignocellulose
US6022419A (en) * 1996-09-30 2000-02-08 Midwest Research Institute Hydrolysis and fractionation of lignocellulosic biomass
US6228177B1 (en) 1996-09-30 2001-05-08 Midwest Research Institute Aqueous fractionation of biomass based on novel carbohydrate hydrolysis kinetics
US5876505A (en) * 1998-01-13 1999-03-02 Thermo Fibergen, Inc. Method of producing glucose from papermaking sludge using concentrated or dilute acid hydrolysis
DK2376642T3 (da) 2008-12-17 2014-01-13 Borregaard As Konvertering af lignocellulosisk biomasse ved forbehandling med sulfit
LT2483331T (lt) 2009-09-29 2017-07-25 Nova Pangaea Technologies Limited Lignoceliuliozinės biomasės frakcionavimo būdas ir sistema
PL3234201T3 (pl) 2014-12-18 2021-02-22 Avantium Knowledge Centre B.V. Sposób wytwarzania stałych sacharydów z wodnego roztworu sacharydów
AU2016353665B2 (en) 2015-11-09 2020-09-10 Avantium Knowledge Centre B.V. Process for the production of a saccharide product from an aqueous solution

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3928121A (en) * 1973-10-23 1975-12-23 Zepeda Castillo Enrique Process for the obtention of fermentable powdered syrup and alphacellulose from xerophyte plants
US4025356A (en) * 1974-01-16 1977-05-24 Anstalt Gemass Method for continuous hydrolysis of pentose containing material and apparatus for implementing the method
US4087316A (en) * 1975-09-02 1978-05-02 Cotton Incorporated Process for obtaining seed hull commodities including cellulosic fibers and xylitol
US4160695A (en) * 1976-07-20 1979-07-10 Projektierung Chemische Verfahrenstechnik Gesellschaft Mit Beschrankter Haftung Process for the production of glucose from cellulose-containing vegetable raw materials
US4138272A (en) * 1977-11-15 1979-02-06 Zepeda Castillo Enrique Process for the obtention of fructose and fructose-rich syrups from xerophyte plants
US4708746A (en) * 1981-12-15 1987-11-24 Werner & Pfleiderer Method the hydrolytic splitting of acid treated comminuted crude cellulose with steam
US4664832A (en) * 1984-09-28 1987-05-12 State Of South Dakota As Represented By The Department Of Transportation Deicing chemicals and their preparation from polysaccharide sources

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CA924713A (en) 1973-04-17
CH485910A (de) 1970-02-15
BR6803218D0 (pt) 1973-01-16
DE1567335A1 (de) 1970-09-03
NL6814849A (xx) 1969-04-21
DE1567335B2 (de) 1978-06-22
GB1228057A (xx) 1971-04-15
AT295435B (de) 1971-11-15
DE1567335C3 (de) 1979-03-29
NL162692C (nl) 1980-06-16
SE355379B (xx) 1973-04-16
LU57096A1 (xx) 1969-01-27
FR1599793A (xx) 1970-07-20
US3787241A (en) 1974-01-22
BE722397A (xx) 1969-04-01
NL162692B (nl) 1980-01-15
FI54507B (fi) 1978-08-31
FI54507C (fi) 1978-12-11

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