US4427453A — Two stage continuous hydrolysis of plant biomass …

Claim 1

Independent Claim 194 words

Process for the continuous hydrolysis of pentosan-containing hemicelluloses, cellulose and corresponding compounds in plant biomass to sugar, in which chopped biomass is subjected in a first stage, in the presence of dilute acid, to temperature and pressure conditions under which the hemicellulose and only partially the cellulose are hydrolyzed during a first reaction time to pentoses and, partially, hexoses, whereupon the pressure of reaction mixture is released and the hydrolysate is separated from the biomass and in which, in at least one further stage, cellulose in the biomass is hydrolyzed during a further reaction time to hexoses in the presence of dilute mineral acid and under more stringent temperature and pressure conditions, whereupon the reaction pressure is released and, the hydrolysate is separated from the remaining biomass, and in which the hydrolysate is further processed, for the production of sugar, wherein the biomass under mechanical pressure is fed into the pressurized reaction chamber while simultaneously substantially removing the air and excess moisture contained in the biomass, the hydrolysis being carried out in a steam vapour phase in the reaction chamber, and in which hydrolysate is separated in several separation steps from the reaction mixture.

Claim 2

Dependent Claim 194 words

Process for the continuous hydrolysis of pentosan-containing hemicelluloses, cellulose and corresponding compounds in plant biomass to sugar, in which chopped biomass is subjected in a first stage, in the presence of dilute acid, to temperature and pressure conditions under which the hemicellulose and only partially the cellulose are hydrolyzed during a first reaction time to pentoses and, partially, hexoses, whereupon the pressure of reaction mixture is released and the hydrolysate is separated from the biomass and in which, in at least one further stage, cellulose in the biomass is hydrolyzed during a further reaction time to hexoses in the presence of dilute mineral acid and under more stringent temperature and pressure conditions, whereupon the reaction pressure is released and, the hydrolysate is separated from the remaining biomass, and in which the hydrolysate is further processed, for the production of sugar, wherein the biomass under mechanical pressure is fed into the pressurized reaction chamber while simultaneously substantially removing the air and excess moisture contained in the biomass, the hydrolysis being carried out in a steam vapour phase in the reaction chamber, and in which hydrolysate is separated in several separation steps from the reaction mixture.

Claim 3

Dependent Claim 44 words

Process according to claim 1 in which the biomass for feeding to the reaction chamber is compressed at least in the volume ratio 1:4 to provide a density of at least 350 kg/m 3 and thereafter is disintegrated by steam used for the reaction.

Claim 4

Dependent Claim 23 words

Process according to claim 1, in which the multistage hydrolysate separation takes place exclusively after the sudden pressure release of the reaction mixture.

Claim 5

Dependent Claim 37 words

Process according to claim 1, in which a hydrolysate separation takes place in at least a first separation stage under the pressure seal of the reaction chamber and the pressure release takes only place after this separation.

Claim 6

Dependent Claim 22 words

Process according to claim 4, in which the hydrolysate separated under pressure seal, separate from solids, is suddenly subjected to pressure release.

Claim 7

Dependent Claim 51 words

Process according to claim 4, in which as separation device for the first separation stage a pressurized separation worm is used, which is connected directly to the exit end of the digester, and that the pressure release of the remaining reaction mixture occurs through the plug tube of the separation worm.

Claim 8

Dependent Claim 29 words

Process according to claim 4, in which a pressure release is followed by further separation stages, in which, as separating device separation worms and/or double wire presses are used.

Claim 9

Dependent Claim 22 words

Process according to claim 7, in which two or more separation stages are carried out by means of a double wire press.

Claim 10

Dependent Claim 74 words

Process according to claim 1, in which the hydrolysate separation after each hydrolysis stage occurs counter current of the hydrolysate, by adding generally fresh water before the last separation stage and by adding in each case the liquid separated in one separation stage before the preceding separation stage whereby the hydrolysate, in case of pressure release between the separation stages, is raised to the higher pressure level for the separation stages before the release.

Claim 11

Dependent Claim 52 words

Process according to claim 1, in which, with the exception of the last hydrolysis stage, in each hydrolysis stage hydrolysate from the next following hydrolysis stage is used as acid-containing dissolution liquid and only the hydrolysate separated in the first separation stage after the first hydrolysis stage is used for further processing.

Claim 12

Dependent Claim 19 words

Process, according to claim 1, in which the hydrolysate of each hydrolysis stage is removed directly for further processing.

Claim 13

Dependent Claim 50 words

Process, according to claim 11, in which the neutralization of the hydrolysate is carried out before or with the pressure release of the corresponding reaction mixture by adding a neutralizer into the outlet end of the horizontal tube digester or into the blow pipe leading to the pressure release chamber.

Claim 14

Dependent Claim 32 words

Process according to claim 4, in which the neutralization of the hydrolysate occurs before the first pressure-sealed separation stage by injecting the neutralizer into the outlet end of the horizontal tube digester.

Claim 15

Dependent Claim 36 words

Process according to claim 1, in which the reaction mixture, even after the pressure release in the reaction chamber, is kept under certain over pressure, to allow use of the steam released by the pressure release.

Claim 16

Dependent Claim 33 words

Process according to any one of claims 1 to 3 in which the chopped biomass is impregnated with acid-containing aqueous dissolution liquid before entry into the filler worm of the first hydrolysis stage.

Claim 17

Dependent Claim 26 words

Process according to any one of claims 1 to 3, in which the acid containing aqueous dissolution liquid is injected directly into the pressurized reaction chamber.

Claim 18

Dependent Claim 31 words

Process according to any one of the claims 1 to 3, in which the biomass is chopped into grain sizes of about 0.1 to 3 mm, preferably 1 to 2 mm.

Claim 19

Dependent Claim 90 words

Process according to any one of claims 1 to 3, in which for further processing of the hydrolysate the neutralized mineral acid is separated from the hydrolysate in the form of a salt of the acid and in which the accumulated remaining biomass consisting mainly of lignin and salt undergo, in the last stage of the process, a two stage combustion in the first stage of which reduction takes place and in the second of which stage, oxidation occurs, in order to recover the mineral acid anhydride and the neutralizer.

Claim 20

Dependent Claim 213 words

Apparatus for the continuous hydrolysis of pentosan-containing hemicelluloses, cellulose and corresponding compounds in plant biomass to sugar in which chopped biomass is treated in a first stage in the presence of dilute acid, at temperatures and pressure conditions under which the hemicellulose and, partially, the cellulose are hydrolyzed during a first reaction to pentoses and partially, hexoses, whereupon the reaction mixture pressure is suddenly released and the hydrolysate is separated from the biomass, and in at least a further stage, cellulose in the biomass is hydrolyzed in the presence of dilute mineral acid and under more severe temperature and pressure conditions, to hexoses, whereupon again the reaction mixture pressure is suddenly released and the hydrolysate is separated from the remaining biomass, and in which the neutralized hydrolysate is further processed for the production of sugars, wherein each hydrolysis stage comprises as reaction chamber, a continuously operating horizontal tube digester containing horizontal conveyor devices, the digester being connected on the entrance side with a conical worm filler with a perforated cone casing for the injection of the biomass and the outlet side is fitted with an outlet device which forms a pressure seal for the exit side of the reaction chamber, and which is connected via a blow pipe with a cyclone-shaped blow tank.

Claim 21

Dependent Claim 213 words

Apparatus for the continuous hydrolysis of pentosan-containing hemicelluloses, cellulose and corresponding compounds in plant biomass to sugar in which chopped biomass is treated in a first stage in the presence of dilute acid, at temperatures and pressure conditions under which the hemicellulose and, partially, the cellulose are hydrolyzed during a first reaction to pentoses and partially, hexoses, whereupon the reaction mixture pressure is suddenly released and the hydrolysate is separated from the biomass, and in at least a further stage, cellulose in the biomass is hydrolyzed in the presence of dilute mineral acid and under more severe temperature and pressure conditions, to hexoses, whereupon again the reaction mixture pressure is suddenly released and the hydrolysate is separated from the remaining biomass, and in which the neutralized hydrolysate is further processed for the production of sugars, wherein each hydrolysis stage comprises as reaction chamber, a continuously operating horizontal tube digester containing horizontal conveyor devices, the digester being connected on the entrance side with a conical worm filler with a perforated cone casing for the injection of the biomass and the outlet side is fitted with an outlet device which forms a pressure seal for the exit side of the reaction chamber, and which is connected via a blow pipe with a cyclone-shaped blow tank.

Claim 22

Dependent Claim 63 words

Apparatus according to claim 19, in which the first separation device for the separation of the hydrolysate in a hydrolysis stage is a worm separator which is directly connected to the outlet end of the tube digester and together with the boiler is under pressure and simultaneously forms the outlet device, and whose perforated cone casing is surrounded by a pressure tight housing.

Claim 23

Dependent Claim 39 words

Apparatus according to claim 20, in which after the worm separator, which is under pressure seal, a blow tank is connected and following that further separation devices are connected in the form of worm separators and/or double wire presses.

Claim 24

Dependent Claim 20 words

Apparatus, according to claim 21, in which the worm separators are essentially of the same construction as the worm filler.

Claim 25

Dependent Claim 35 words

Apparatus according to claim 22, in which in the case of a further separation stage, the worm filler for the following tube boiler may simultaneously serve as a last separation device of the previous stage.

Claim 26

Dependent Claim 39 words

Apparatus according to claim 21, in which the further separation devices consist of at least a double wire press which is fitted with two press stretches with separated hydrolysate collection devices for the execution of a two-stage hydrolysate separation.

Claim 27

Dependent Claim 24 words

Apparatus according to claim 24, in which a feeder device is provided between the two press to feed fresh water or hydrolysate-containing wash water.

Claim 28

Dependent Claim 20 words

Apparatus according to claim 19, in which the plug tube of the worm filler opens directly in the digester tube.

Claim 29

Dependent Claim 28 words

Apparatus according to claim 26, in which directly after the exit end of the plug tube in the inner space of the digester, steam injection devices are positioned.

Claim 30

Dependent Claim 43 words

Apparatus according to claim 26 or 27, in which the ratio of length to diameter of the plug tube is at least 2:1 and the volume compression ratio of the worm from the worm entry to the plug tube is at least 1:4.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1987-01-23	1987-07-25	1988-01-24	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1991-01-23	1991-07-25	1992-01-24	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1995-01-23	1995-07-25	1996-01-24	$7700.00	Window Closed / Lapsed

Two stage continuous hydrolysis of plant biomass to sugars

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