Cellulose Material Patents (Class 127/37)
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Patent number: 4681935Abstract: The invention concerns a procedure for recovery of soluble carbohydrates present in wood, in connection with the alkaline cellulose digesting process. According to the invention, recovery of carbohydrates takes place at the initial phase of the cellulose digesting process, where the digesting solution contains dissolved polysaccharides in abundance, while the content of polymeric lignin in the solution is low. A situation like this exists at the stage when the digesting solution has not yet reached the temperature at which the digestion process mainly takes place. As taught by the invention, the carbohydrates are recovered by conducting digesting solution to an ultrafilter, which separates the carbohydrates therefrom, and by returning the filtered solution to the cellulose digestion. The carbohydrates that are obtained may be used e.g. in the manufacturing of sugar alcohols, or as raw materials for biotechnical processes.Type: GrantFiled: November 27, 1985Date of Patent: July 21, 1987Assignee: Enso-Gutzeit OyInventors: Kaj Forss, Matti Sten, Juhani Peltonen, Veikko Jokela
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Patent number: 4668340Abstract: A method and apparatus are provided for the treatment of comminuted cellulosic fibrous material to effect prehydrolysis, and then subsequently kraft digestion, thereof, to produce paper pulp. The material is steamed, entrained in liquid to form a suspension, and transferred by a high pressure feeder in a first circulation loop to the top of a first vertical vessel. At the top of the vessel, a liquid/solids separator is provided, and the liquid withdrawn from the top of the first vessel into the return conduit of the first circulation loop includes recoverable hydrolysate (which contains hemicellulose, sugars, and the like). In the first vessel, countercurrent acid hydrolysis takes place in the top of the vessel, and a countercurrent wash is effected in the bottom of the vessel. A part of the liquid in the return conduit of the first circulatory loop is diverted to one or more flash tanks, to produce steam and a liquid with a high concentration of hydrolysate.Type: GrantFiled: March 20, 1984Date of Patent: May 26, 1987Assignee: Kamyr, Inc.Inventor: Michael I. Sherman
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Patent number: 4664717Abstract: Polysaccharides are at least partially hydrolyzed by contact with a composition containing urea, sulfuric acid, and water in which the urea/sulfuric acid molar ratio is less than 2. Such proportions of urea and sulfuric acid assure the presence of the monourea adduct of sulfuric acid. The polysaccharide can be hydrolyzed to an extent sufficient only to hydrate the polysaccharide to produce a hydrated polysaccharide such as hydrated cellulose, or it can be completely hydrolyzed to its constituent monosaccharides. Thus, cellulose can be converted to glucose.Type: GrantFiled: November 20, 1984Date of Patent: May 12, 1987Assignee: Union Oil Company of CaliforniaInventor: Donald C. Young
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Patent number: 4650689Abstract: A method for producing a fermentable wort useful to produce ethanol from cellulosic materials is particularly adaptable for batch-wise processing. The broad method includes the steps of placing the materials in an airtight vessel that is evacuated to a moderate vacuum at a reduced temperature of 20.degree. C. or less. Highly concentrated mineral acid gas, such as HCl, is introduced to raise the vessel pressure to a pressure less than 1500 mm of Hg wherein the concentration of acid gas is at least 40%. These temperatures and pressures are maintained for at least 30 minutes to depolymerize the cellulose after which the vessel is again evacuated to remove the excess gas and then raised to ambient pressure so that the material is removed. The depolymerized material, which contains some adsorbed acid gas, is mechanically conveyed against a counterflow of hot water.Type: GrantFiled: March 25, 1985Date of Patent: March 17, 1987Assignee: Urban Fuels, Inc.Inventor: William S. Hedrick
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Patent number: 4649113Abstract: By treating agricultural crop residues and other nonwoody lignocellulosic plant substrates with H.sub.2 O.sub.2 at a controlled pH within the range of about 11.2 to 11.8, the substrates are partially delignified and unprecedented levels of the cellulose and hemicellulose as insoluble fractions are made available for subsequent use. The products of this treatment are nontoxic and are characterized by low crystallinity and near quantitative cellulase digestibility. They are useful as carbohydrate sources in ruminant feeds and as microbial feedstocks for commercial process such as the production of alcohol and generation of single-cell protein.Type: GrantFiled: December 28, 1983Date of Patent: March 10, 1987Assignee: The United States of America as represented by the Secretary of AgricultureInventor: John M. Gould
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Method of producing level off DP microcrystallinecellulose and glucose from lignocellulosic material
Patent number: 4645541Abstract: Microcrystalline cellulose has many applications in the pharmaceutical, food, paper and structural composite industries. Level off DP (Degree of Polymerization) microcrystalline cellulose is made up of a chain of about 250 glucose molecules in the form of microcrystal. In nature, several microcrystals are hinged together and surrounded by amorphous cellulose to form a cellulose microfibril. If the amorphous cellulose is removed, the resultant product is called level off DP (Degree of Polymerization) microcrystalline cellulose. When lignocellulosic material is processed according to applicant's earlier processes (Canadian Pat. Nos. 1,096,374 and 1,141,376), the dissociated material is partitioned by removing the lignin and the xylan leaving a low DP (320) cellulose fraction.Type: GrantFiled: December 4, 1985Date of Patent: February 24, 1987Inventor: Edward A. DeLong -
Patent number: 4645658Abstract: A method of recovering concentrated hydrochloric acid from the product obtained from the acid hydrolysis of a cellulose containing material such as biomass. The method involves contacting such product with an extracting solvent, of which a major portion is acetophenone, to separate the product into a hydrochloric acid enriched phase and a hydrochloric acid depleted phase and then separating and recovering the hydrochloric acid from the hydrochloric acid enriched phase.Type: GrantFiled: April 30, 1985Date of Patent: February 24, 1987Inventors: James L. Gaddy, Edgar C. Clausen
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Patent number: 4642287Abstract: An improved process for pretreating biomasses in advance of their enzymatic treatment is provided which process comprises subjecting a biomass together with an aqueous solution of an alkaline compound to kneading and reaction in a biaxial extruder, and which process has advantages that a continuous treatment in a very short time is possible, and the heat quantity required for the pretreatment is greatly reduced.Type: GrantFiled: April 5, 1984Date of Patent: February 10, 1987Assignee: Shinnenryoyu Kaihatsugijutsu KenkyukumiaiInventors: Takeshi Inoi, Toshiaki Akabane, Yasuhiro Kurokawa, Shingo Matsuoka
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Patent number: 4637835Abstract: A method of hydrolyzing cellulose to glucose and other saccharides, involving the bringing together in a reaction area an alphacellulose containing material, water, an effective amount of a calcium chloride catalyst and a minor amount of a hydrogen ion in a feedstock. The temperature of the feedstock is adjusted to between 150.degree. C. to 250.degree. C. at a pressure of at least 160 psig for a retention time of at least 20 seconds in the reaction area to convert the alphacellulose to said glucose and other saccharides.Type: GrantFiled: June 28, 1985Date of Patent: January 20, 1987Assignee: Power Alcohol, Inc.Inventor: Richard T. Nagle
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Patent number: 4629575Abstract: Circulating and non-circulating well-drilling fluids are provided comprising parenchymal cell cellulose. In accordance with a preferred embodiment, improved viscosity and fluid loss control in circulating well-drilling fluids are obtained from the inclusion of parenchymal cell cellulose in such fluids. In accordance with another preferred embodiment, certain polymers, especially anionic polymers, and polymers derived from hemicellulosic materials are admixed with parenchymal cell cellulsoe in well fluids to provide synergistic fluid loss control and other beneficial properties. Methods for the employment of circulating and non-circulating well fluids employing parenchymal cell cellulose are also disclosed.Type: GrantFiled: July 6, 1983Date of Patent: December 16, 1986Assignee: SBP, Inc.Inventor: Michael K. Weibel
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Patent number: 4615742Abstract: A progressive batch hydrolysis process for producing sugar from a lignocellulosic feedstock, comprising passing a stream of dilute acid serially through a plurality of percolation hydrolysis reactors charged with said feedstock, at a flow rate, temperature and pressure sufficient to substantially convert all the cellulose component of the feedstock to glucose; cooling said dilute acid stream containing glucose, after exiting the last percolation hydrolysis reactor, then feeding said dilute acid stream serially through a plurality of prehydrolysis percolation reactors, charged with said feedstock, at a flow rate, temperature and pressure sufficient to substantially convert all the hemicellulose component of said feedstock to glucose; and cooling the dilute acid stream containing glucose after it exits the last prehydrolysis reactor.Type: GrantFiled: January 10, 1985Date of Patent: October 7, 1986Assignee: The United States of America as represented by the Department of EnergyInventor: John D. Wright
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Patent number: 4612286Abstract: A method of treating biomass having fermentable material is provided utilizing acid hydrolysis in a countercurrent diffusion treatment structure. By practicing the invention acid usage is minimized, pentose concentration in the hydrolysate solution is maximized, and ethanol, butanol, butanediol, and the alcohols can be produced without the input of any external energy whatsoever into the production method. Biomass is particlized and slurried, and then is continuously subjected to acid hydrolysis at temperature, acid concentration, and residence time conditions sufficient to effect hydrolysis of the hemicellulose in the biomass to effect separation of pentose and hexose sugars into a hydrolysate having insufficient furfural to substantially inhibit fermentation microorganism growth, while not substantially hydrolyzing the cellulose in the biomass.Type: GrantFiled: July 23, 1984Date of Patent: September 16, 1986Assignee: Kamyr, Inc.Inventors: Michael I. Sherman, Carl L. Elmore
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Patent number: 4608245Abstract: A method of recovering concentrated sulfuric acid from the product obtained from the acid hydrolysis of a cellulose-containing material such a biomass. The method involves contacting the product with an extraction solvent comprising one or more of the C.sub.4 -C.sub.7 alcohols as the major component to separate the product into a sulfuric acid enriched phase. The sulfuric acid from this enriched phase is then separated and recovered by a further extraction procedure.Type: GrantFiled: October 17, 1985Date of Patent: August 26, 1986Inventors: James L. Gaddy, Edgar C. Clausen
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Patent number: 4591386Abstract: A process and apparatus for the acid hydrolysis of waste cellulose to glucose of the type wherein waste cellulose is continuously fed into an inlet port of a twin screw extruder, water is continuously fed into reaction zone in the extruder, downstream of the inlet port, the cellulose is continuously reacted with water in the presence of an acid catalyst at elevated temperature and pressure in the reaction zone while being continuously conveyed to an outlet port of the extruder having a given diameter and the reacted cellulose is discharged from the extruder while the elevated temperature and pressure in the reaction zone is maintained. The elevated pressure is maintained by forming a dynamic seal zone at the upstream end of the reaction and continuously discharging the reacted material downstream of the outlet port at a predetermined volume rate of flow to maintain the pressure by passing the discharge through an orifice pipe having a smaller diameter than the given diameter of the outlet port.Type: GrantFiled: March 25, 1983Date of Patent: May 27, 1986Assignee: New York UniversityInventors: Barry Rugg, Robert Stanton
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Patent number: 4591388Abstract: A process for the separation of arabinose is disclosed which comprises the selective adsorption of same on BaX zeolitic molecular sieves. The process is especially useful for separating arabinose from mixtures of sugars containing arabinose.Type: GrantFiled: May 6, 1985Date of Patent: May 27, 1986Assignee: Union Carbide CorporationInventors: Chien C. Chao, John D. Sherman
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Patent number: 4589924Abstract: The semi-continuous process according to the invention for hydrolyzing cellulose-containing material (substrate) with gaseous hydrogen fluoride comprises sorption and subsequent desorption of HF in a total of n steps. The substrate is divided into n batches in n reactors (1a, 1b, 1c, . . . ); each batch passes through the n process steps in one reactor (1a, . . . ). Initially, sorption is carried out in the first to the (n/2)th step by the action of HF-inert gas mixtures, having an HF concentration which increases from sorption step to sorption step, at a temperature above the boiling point of HF. Subsequently, desorption is brought about in the ((n/2)+1)th to nth step by treating with heated HF-inert gas mixtures having an HF concentration which decreases from desorption step to desorption step; n is an even number from 4 to 12 and the n steps each take place in the same time segments (periods). The sequence of steps is displaced by one period from each batch to the next batch.Type: GrantFiled: March 12, 1985Date of Patent: May 20, 1986Assignee: Hoechst AktiengesellschaftInventors: Rudiger Erckel, Raimund Franz, Rolf Woernle, Theodor Riehm
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Patent number: 4579595Abstract: A moist ligno-cellulosic mass was impregnated under cooling with HCl gas then it was warmed up in order to cause said mass to hydrolyze and the excess of acid to escape, the brewing action consecutive to said desorption improving the efficiency of said hydrolysis.Type: GrantFiled: May 16, 1985Date of Patent: April 1, 1986Assignee: Battelle Memorial InstituteInventors: Jean-Pierre Sachetto, Jean-Michel Armet, Ake A. Johansson, Alain Roman, Sergio Cuccolo
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Patent number: 4564595Abstract: A continuous process for the production of alcohol, preferably ethanol, from cellulosic materials. The cellulosic materials are delignified such that the hemicellulose and the cellulose can be subsequently acid hydrolyzed into simple sugars. These sugars are fermented in the presence of yeast to yield ethanol and carbon dioxide. The alcohol vapor is removed from the fermentation solution under a reduced pressure and subsequently distilled. Carbon dioxide gas may be sparged throughout the fermenting solution in order to aid in the removal of the alcohol from the fermenting solution. The gaseous carbon dioxide is captured and utilized in the manufacture of additional quantities of ethanol or other basic chemicals.Type: GrantFiled: January 9, 1984Date of Patent: January 14, 1986Assignee: Biomass International Inc.Inventor: Alan M. Neves
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Patent number: 4556431Abstract: A continuous process for hydrolyzing cellulose-containing material (substrate) with gaseous hydrogen fluoride, HF is sorbed by the substrate at a temperature above its boiling point in n sorption steps and thereafter the sorbed HF is removed from the substrate by heating in n desorption steps. The number n of sorption steps and of desorption steps is identical and the reaction steps mentioned each occur in reactors which are separated from one another in a gas-tight manner. After introduction into the first sorption reactor (1a), the substrate passes consecutively through gas-tight valves into the second (1a) . . . nth sorption reactor and from the latter, optionally via a hold-up reactor (2) into the first, second, . . . nth desorption reactor (3a) and is removed from the nth desorption reactor (3a). The streams of HF gas, which contain an inert carrier gas in addition to HF, are circulated between the first (1a) or second (1b) or . . . (n-1)th or nth sorption reactor and the nth (3a) or (n-1)th (3b) . . .Type: GrantFiled: February 28, 1985Date of Patent: December 3, 1985Assignee: Hoechst AktiengesellschaftInventors: Rudiger Erckel, Raimund Franz, Rolf Woernle, Theodor Riehm
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Patent number: 4556430Abstract: A process for hydrolysis of biomass wherein the biomass is mixed with a small amount of an aqueous acid to produce a wet meal. A non-aqueous carrier fluid is used to form a slurry of the biomass, and the temperature and pressure are established at appropriate levels to effect hydrolysis of the biomass to decomposition products that include sugar for a time period that is sufficient for the hydrolysis to occur.Type: GrantFiled: November 5, 1984Date of Patent: December 3, 1985Assignee: Trustees of Dartmouth CollegeInventors: Alvin O. Converse, Hans E. Grethlein
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Patent number: 4556432Abstract: The continuous process for hydrolyzing cellulose-containing material (substrate) is carried out by sorption of gaseous HF in a sorption reaction (1) and subsequent desorption in n steps, which are carried out in n reactors which are separated from one another in a gas-tight manner. The substrate is introduced via a gas-tight valve into the sorption reactor (1), passes through this and then reaches consecutively, through gas-tight valves, a hold-up reactor (2) and the first (3c), second (3b), . . . nth desporption reactor, from which it is then removed. The desorption is carried out in each case by the action of one of the n inert gas streams on the substrate at different temperatures, the particular inert gas stream being enriched with the HF being liberated during desorption.Type: GrantFiled: March 12, 1985Date of Patent: December 3, 1985Assignee: Hoechst AktiengesellschaftInventors: Rudiger Erckel, Raimund Franz, Rolf Woernle, Theodor Riehm
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Patent number: 4525218Abstract: Cellulose is selectively hydrolyzed to glucose without the formation of degradation by-products by pretreating the cellulose to form soluble cellodextrins through treatment with concentrated (60-80%) solutions of zinc chloride. Zinc chloride is then separated from the mixture by extraction with attendant precipitation of the cellodextrin material which is the hydrolyzed, chemically or enzymatically to glucose.Type: GrantFiled: May 11, 1982Date of Patent: June 25, 1985Assignee: Purdue Research FoundationInventors: Li F. Chen, Che-Ming Yang
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Patent number: 4520105Abstract: A process for the production of sugars, and optionally cellulose and lignin, from lignocellulosic vegetable materials which comprises subjecting the vegetable materials to a chemical pretreatment with a mixture of water and lower aliphatic alcohols and/or ketones at a temperature from 100.degree. to 190.degree. C. for a period of from 4 hours to 2 minutes with control of the breakdown of the hemicellulose components followed by separation of residue and a subsequent main chemical treatment with a similar solvent mixture at elevated temperatures for a further period of from 6 hours to 2 minutes.Type: GrantFiled: August 10, 1983Date of Patent: May 28, 1985Assignee: Bau- und Forschungsgesellschaft Thermoform AGInventors: Michael Sinner, Hans-Hermann Dietrichs, Jurgen Puls, Werner Schweers, Karl-Heinz Brachthauser
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Patent number: 4516566Abstract: A process for the separation of arabinose is disclosed which comprises the selective adsorption of same on BaX zeolitic molecular sieves. The process is especially useful for separating arabinose from mixtures of sugars containing arabinose.Type: GrantFiled: December 30, 1982Date of Patent: May 14, 1985Assignee: Union Carbide CorporationInventors: Chien C. Chao, John D. Sherman
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Patent number: 4511433Abstract: A method for delignifying ligno-cellulosic materials and efficiently separate from each other the constituents thereof. Said materials are heated in an aqueous acid medium in the presence of phenol compounds. Then the reaction medium is drained and washed for isolating the purified solid cellulose pulp, the liquid phase separating into two layers: an aqueous layer rich with pentoses and an organic layer rich with phenols and lignin, the latter providing, by distillation and pyrolysis of the residue, a quantity of phenols at least equal to that of the phenols used in the delignification stage.Type: GrantFiled: July 27, 1984Date of Patent: April 16, 1985Assignee: Battelle Memorial InstituteInventors: Herve Tournier, Allan A. Johansson, Jean-Pierre Sachetto, Jean-Michel Armanet, Jean-Pierre Michel, Alain Roman
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Patent number: 4508745Abstract: A method of hydrolyzing a coffee extraction residue material to produce a mannan oligomer solution having oligomers from DP 1 to DP 10 is disclosed. The coffee material, preferably spent grounds from a commercial percolation system, is hydrolyzed in a reactor in the presence of an acid catalyst. A tubular plug flow reactor is convenient, although any reactor providing for the relatively high temperature, short time reaction will suffice. Particular acid catalysts include sulphuric acid, phosphoric acid, acetic acid and carbon dioxide gas. Depending on the specific time, temperature and catalyst concentration selected, a mannan oligomer solution having any desired distribution of oligomers between DP 1 and DP 10 is produced.Type: GrantFiled: December 30, 1982Date of Patent: April 2, 1985Assignee: General Foods CorporationInventors: Charles V. Fulger, Howard D. Stahl, Evan J. Turek, Renee Bayha
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Patent number: 4478644Abstract: Process and device for hydrolyzing cellulose material in an extruder with two parallel screws in which the material introduced in the moist condition and, transported by the screws is malaxated, heated to a temperature of above 200.degree. C. in the downstream part of the extruder where it is contacted with an acid solution and progressively compressed, to a pressure higher than the saturated vapor pressure of the liquid phase of the hydrolyzed material at the temperature reached in the downstream part and maintained by a control device for the evacuation of the material.Type: GrantFiled: April 15, 1983Date of Patent: October 23, 1984Assignee: Creusot-LoireInventors: Pierre Berger, Maurice Gelus
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Patent number: 4470851Abstract: Comminuted cellulosic materials which may or may not contain lignin are partially or totally hydrolyzed or saccharified by an improved organosolv process using an aqueous acetone solvent mixture containing a small amount of an acidic compound and containing at least about 70 percent by volume of acetone and up to virtually anhydrous acetone. The process is performed at elevated reaction temperatures, preferably at 145.degree. C. to 230.degree. C., for a limited period of time and then with cooling such that the resultant dissolved sugars from the hydrolysis are not degraded into non-sugars. In particular the reaction is conducted such that the cellulosic material is dissolved and such that at least ninety percent or more of available sugars in the cellulosic material are recovered. Unexpectedly it has been found that acetone at high concentration forms stable complexes with the sugars which prevents their degradation and also facilitates separation of the sugars.Type: GrantFiled: February 9, 1982Date of Patent: September 11, 1984Inventors: Laszlo Paszner, Pei-Ching Chang
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Patent number: 4468256Abstract: A process for the hydrolysis of cellulose from vegetable raw materials to glucose, particularly using wood as the raw material, comprises conveying the raw material through a hydrolysis zone in finely comminuted form, the raw material being impregnated with dilute acid and at a sufficiently high hydrolysis temperature. The raw material impregnated with dilute acid is supplied in portions and continuously through the hydrolysis zone where it is heated to a hydrolysis temperature of above 250.degree. C. by means of high pressure steam. This takes place in an extremely short time accompanied by a sudden pressure rise.Apparatus for performing this process comprises a tubular reactor having at least one straight pipe through which can be conveyed an endless piston chain. The pistons of this chain form a leakage gap opposite the inner wall of the pipe and, in each case, two adjacent pistons define a piston chamber. A high pressure steam line is arranged to issue approximately into the center of the pipe.Type: GrantFiled: December 15, 1981Date of Patent: August 28, 1984Assignee: Werner & PfleidererInventor: Klaus-Jurgen Hinger
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Patent number: 4461648Abstract: This invention comprises a method for increasing the accessibility of cellulose in lignocellulosic materials to chemical or biochemical reagents. The material is steam cooked for a predetermined time, then rapidly depressurized. A venting sequence is used to remove volatiles from the reactor. Optimal cooking times for normal and acid catalyzed cooking are disclosed, according to the discovery of a novel set of governing equations, wherein optimum cooking times can be determined as a time integration of reactor pressure.Type: GrantFiled: June 1, 1981Date of Patent: July 24, 1984Inventor: Patrick Foody
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Patent number: 4452640Abstract: Cellulose may be quantitatively hydrolyzed to glucose without formation of degradation products by pretreatment of cellulose with zinc chloride to liquify the cellulose and thereafter hydrolyzing the cellulose with acid.Type: GrantFiled: May 11, 1982Date of Patent: June 5, 1984Assignee: Purdue Research FoundationInventors: Li Fu Chen, Che-Ming Yang
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Patent number: 4432805Abstract: A method for continuous saccharification of plant raw material by feeding the raw material as such or prehydrolyzed and a dilute sulphuric acid solution into a flow reactor in order to hydrolyze the raw material under pressure and at a high temperature, discharging dry solids and liquid from the reactor by expansion and separating liquid and solids, wherein the raw material and sulfuric acid solution are led through the reactor at equal rate, which is the same as required by the more easily hydrolyzable particles of the raw material, the solids and liquid together are discharged into the same blow tank and at least part of the separated coarse solid is returned into the reactor.Type: GrantFiled: June 23, 1982Date of Patent: February 21, 1984Assignee: Oy Tampella ABInventors: Antti I. Nuuttila, Veikko J. Pohjola
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Patent number: 4427584Abstract: A process which comprises a stepwise treatment of natural fibers with liquid or gaseous sulphur trioxide to cause decrystallization of the alpha-cellulose therein, followed by hydrolysis of the treated fibers to produce (1) an aqueous solution of hexose sugars which can be utilized as feedstock when using a yeast organism to produce ethanol, (2) pentose sugars that may be used as a syrup for feed to ruminants, and (3) a residual lignin fraction that may be used as fuel to energize said process.Type: GrantFiled: May 5, 1982Date of Patent: January 24, 1984Assignee: University of FloridaInventors: Ferdinand LeGrand, Seymour S. Block
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Patent number: 4427453Abstract: Process and apparatus for the continuous hydrolysis of plant biomass containing cellulose and hemicellulose.Type: GrantFiled: October 15, 1981Date of Patent: January 24, 1984Inventor: Franz J. Reitter
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Patent number: 4421856Abstract: The yield of fermentable sugar, largely glucose (dextrose), resulting from the acid catalyzed hydrolysis of a carbohydrate polymer such as starch or cellulose can be significantly increased by the addition to the hydrolysate under acid hydrolysis conditions of water soluble non-fermentable carbohydrate such as stillage recovered from a downstream ethanol distillation facility.Type: GrantFiled: November 12, 1981Date of Patent: December 20, 1983Assignee: National Distillers and Chemical CorporationInventors: Werner C. Muller, Franklyn D. Miller
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Patent number: 4409032Abstract: Cellulose-containing material is rapidly saccharified to convert pentosans and hexosans to sugars by cooking under pressure at from 180.degree. C. to 220.degree. C. with acetone-water solvent mixture carrying from 0.05 to 0.25 weight percent of phosphoric, sulfuric or hydrochloric acids.A predominantly cellulosic material, e.g. a delignified pulp, is hydrolysed to yield relatively pure glucose recoverable from liquor which is flowed through the cellulose, then withdrawn and cooled and neutralized within an elapsed time of a minute or less.Whole wood is nearly totally dissolvable by the process, yielding mixed pentoses and hexoses. The dehydration and degradation products of sugars are formed by prolonging retention time of liquor from 20 to 45 minutes.Type: GrantFiled: March 26, 1981Date of Patent: October 11, 1983Assignee: Thermoform Bau-Und ForschungsgesellschaftInventors: Laszlo Paszner, Pei-Ching Chang
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Patent number: 4400218Abstract: Glucose-containing products can be manufactured in apparatus comprising a continuous screw conveyor member rotatable in a continuous press cylinder having three regions in cascade arrangement between an intake opening and an output opening. The regions comprise an intake region for the rapid and economical intake of different kinds of products, a compression region for building up a very high pressure of from about 20 to 300 bars for disintegrating the products and for heating the product by intensive shearing thereof to a temperature of up to 250.degree. C., and a catalyst injection region for intensive action on and mixing or hydrolysis of the cellulosic substances with trifluoroacetic acid or the like injected through nozzles.Type: GrantFiled: March 5, 1982Date of Patent: August 23, 1983Assignee: Hermann Berstorff Maschinenbau GmbHInventors: Klaus Koch, Gerhard Syrbius
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Patent number: 4400468Abstract: A process is provided for producing adipic acid from a renewable resource, i.e., biomass. The process comprises: hydrolyzing the renewable resource to provide 5-hydroxymethylfurfural, hydrogenating the 5-hydroxymethylfurfural in the presence of a catalyst to provide 2, 5-tetrahydrofurandiomethanol, treating the 2, 5-tetrahydrofurandiomethanol with hydrogen in the presence of a catalyst to provide 1, 6 hexanediol, and oxidizing the 1, 6 hexanediol in the presence of a microorganism to provide adipic acid. The formation of the adipic acid is provided with the microorganism of Gluconobacter oxydans subsp. oxydans. The renewable resources are wastes selected from the group consisting of paper, wood, corn stalks, and logging residues.Type: GrantFiled: October 5, 1981Date of Patent: August 23, 1983Assignee: Hydrocarbon Research Inc.Inventor: Marcel Faber
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Patent number: 4395543Abstract: Cellulosic products having a high hemicellulose to lignin weight ratio are obtained by extracting a cellulosic composition with basic ethanol-water solution having a pH between about 12 and about 14 at a temperature between about 15.degree. and about 70.degree. C. and for a time period between about 2 and about 80 hours.Type: GrantFiled: August 12, 1981Date of Patent: July 26, 1983Assignee: Massachusetts Institute of TechnologyInventors: Daniel I. C. Wang, George C. Avgerinos
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Patent number: 4390375Abstract: A process and apparatus for the acid hydrolysis of waste cellulose to glucose of the type wherein waste cellulose is continuously fed into an inlet port of a twin screw extruder, water is continuously fed into reaction zone in the extruder, downstream of the inlet port, the cellulose is continuously reacted with water in the presence of an acid catalyst at elevated temperature and pressure in the reaction zone while being continuously conveyed to an outlet port of the extruder having a given diameter and the reacted cellulose is discharged from the extruder while the elevated temperature and pressure in the reaction zone is maintained. The elevated pressure is maintained by forming a dynamic seal zone at the upstream end of the reaction and continuously discharging the reacted material downstream of the outlet port at a predetermined volume rate of flow to maintain the pressure by passing the discharge through an orifice pipe having a smaller diameter than the given diameter of the outlet port.Type: GrantFiled: April 17, 1981Date of Patent: June 28, 1983Assignee: New York UniversityInventors: Barry Rugg, Robert Stanton
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Patent number: 4384897Abstract: Method of treating biomass material wherein it is subjected to two stage hydrolysis in which in first stage, the more easily hydrolyzed polysaccharides, such as hemicelluloses, are depolymerized and in second stage the more difficultly depolymerizable material, e.g., cellulose, is depolymerized. The biomass material is preferably subjected to a sensitization step between the first and second hydrolyzing stages by contact with molecular oxygen.Type: GrantFiled: November 23, 1981Date of Patent: May 24, 1983Assignee: The Regents of the University of CaliforniaInventor: David L. Brink
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Patent number: 4378432Abstract: Sweetened liquors are obtained from a cellulose-containing vegetable substrate by a process comprising two essential steps:(a) treating the vegetable substrate with an aqueous solution of phosphoric acid alone or in admixture with sulfuric acid, and(b) thereafter effecting enzymatic hydrolysis of the resultant treated substrate to recover additional reducing sugars.Type: GrantFiled: September 25, 1981Date of Patent: March 29, 1983Assignee: Institut Francais du PetroleInventors: Michele Castelli, Odile Chaude, Jean-Paul Vandecasteele
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Patent number: 4370172Abstract: Method and apparatus for feeding vegetable material into a reaction vessel nder pressure to subject the vegetable material to a reaction such as cooking or hydrolysis. The vegetable material is shredded and impregnated with a treating liquid. The resulting liquid-solid mixture is fed by a vortex pump to the reaction vessel. Rate of flow to the reaction vessel is controlled by a flow meter and a variable-speed motor driving the vortex pump.Type: GrantFiled: March 17, 1981Date of Patent: January 25, 1983Assignee: Compagnie de Construction Mecanique Sulzer, French Societe AnonymeInventor: Charles Gueissaz
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Patent number: 4359532Abstract: An improved method suitable for extracting glucose from green crops, such as leaves, grasses, legumes, stems of green plants and tree leaves. The method comprises the steps of subjecting the green crops to a pulping action in an organic acid solution recirculated from a subsequent fermentation separation step to produce a pulp comprising a protein-rich liquid and fibrous material, separating protein-rich liquid in the pulp from the fibrous material and separating protein from the protein-rich liquid by initiating anaerobic fermentation in an acidic solution thereby providing a concentrated protein fraction suitable for preservation and an acidic solution. At least a portion of the acidic solution is recycled to the separation step, the recycling of the solution being provided for purposes of washing the fibrous material to remove residual protein therefrom.Type: GrantFiled: September 8, 1980Date of Patent: November 16, 1982Assignee: Aluminum Company of AmericaInventor: Melvin H. Brown
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Patent number: 4350766Abstract: A method for the production of pentose syrup from hemicellulosic material comprising the separate steps of:(a) mixing said hemicellulose material with an acid selected from the group consisting of sulfuric and hydrochloric to obtain a final concentration of from about 1% to 15% at liquid:solid ratios between 0.1 and 4.0 whereby the material is ready for hydrolyzing directly or being stored for an indefinite period of time at ambient temperatures without degradation;(b) hydrolyzing the acidified material from step (a) by heating the material to a reaction temperature of from 90.degree. to 120.degree. C. for a period of time sufficient to hydrolyze substantially all of the hemicellulose;(c) leaching the hydrolyzed material at a temperature of from about 15.degree. to 100.degree. C. with an aqueous medium by percolating said medium through the hydrolyzed material at a velocity of 0.016 to 0.Type: GrantFiled: August 1, 1980Date of Patent: September 21, 1982Assignee: Purdue Research FoundationInventor: Robert L. Mehlberg
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Patent number: 4342831Abstract: Method of preconditioning acid hydrolyzates derived from lignocellulosic materials such as sawdust or newspaper and preconditioned acid hydrolyzates are provided. The preconditioning negates the effect of substances which tend to inhibit fermentation and comprises a series of steps including steam-stripping, calcium oxide treatment at a pH of 10 to 10.5, adjusting the pH to about 6 to 7 with a mineral acid and especially phosphoric acid and concentrating the hydrolyzate solution to a glucose concentration of less than 150 grams per liter. Glucose contained in such preconditioned hydrolyzates is readily fermentable to ethyl alcohol, in theoretical yield, after fermentation for as short a period as 1 to 2 hours.Type: GrantFiled: April 9, 1981Date of Patent: August 3, 1982Assignee: American Can CompanyInventors: Marcel D. Faber, Richard H. Ernst, Philip H. Lefebvre
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Patent number: 4334026Abstract: A hybrid bio-thermal liquefaction process for improved carbonaceous liquefaction to produce alcohol containing fuels wherein an organic carbonaceous feed is subjected to active fermentation producing alcohol containing liquid fuel product and fermentation residue, the fermentation residue being introduced into a thermochemical converter and at least a substantial portion of the organic carbon component of the residue converted under elevated temperature conditions producing thermochemical converter products and thermochemical residue with a portion of at least one of the thermochemical products or their derivatives, or thermochemical residue being passed to the fermentation reactor. The process provides high overall process energy efficiencies and utilizes the total agricultural biomass crop thereby greatly reducing waste disposal problems.Type: GrantFiled: September 11, 1980Date of Patent: June 8, 1982Assignee: Institute of Gas TechnologyInventors: David P. Chynoweth, Paul B. Tarman
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Patent number: 4316747Abstract: A process and apparatus for the conversion of waste cellulose to glucose wherein an aqueous slurry of waste cellulose is acid hydrolyzed includes continuously feeding an aqueous slurry of waste cellulose into an inlet port with a twin screw extruder, continuously reacting the cellulose with water in the presence of an acid catalyst at elevated temperature and pressure in a reaction zone disposed in the extruder between the inlet port and an outlet port while continuously conveying same to the outlet port and at least quasi-continuously discharging the reacted cellulose from the extruder while maintaining the elevated temperature and pressure in the reaction zone by forming a dynamic seal zone at the upstream end of the reaction zone and valving the discharge downstream of the outlet port.Type: GrantFiled: March 18, 1980Date of Patent: February 23, 1982Assignee: New York UniversityInventors: Barry A. Rugg, Walter Brenner
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Patent number: 4316748Abstract: A process and apparatus for the acid hydrolysis of waste cellulose to glucose of the type wherein waste cellulose is continuously fed into an inlet port of a twin screw extruder, water is continuously fed into reaction zone in the extruder downstream of the inlet port, the cellulose is continuously reacted with water in the presence of an acid catalyst at elevated temperature and pressure in the reaction zone while continuously conveying same to an outlet port of the extruder and the reacted cellulose is discharged from the extruder the elevated temperature and pressure in the reaction zone is maintained, has the elevated pressure is maintained by forming a dynamic seal zone at the upstream end of the reaction zone by providing an unthreaded and radially recessed discontinuity in the screws.Type: GrantFiled: March 18, 1980Date of Patent: February 23, 1982Assignee: New York UniversityInventors: Barry A. Rugg, Robert Stanton
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Patent number: 4314854Abstract: A method to enhance the reactivity of cellulose-containing materials to cellulase enzymes by treating an aqueous suspension of the material with hydrogen peroxide in the presence of a Mn.sup.+2 ion forming manganese compound.Type: GrantFiled: March 5, 1981Date of Patent: February 9, 1982Assignee: Bio Research Center Company Ltd.Inventor: Motoyoshi Takagi