Method for continuous countercurrent ogranosolv saccharification of comminuted lignocellulosic materials

• US 4,941,944 A
• Filed: 01/02/1990
• Issued: 07/17/1990
• Est. Priority Date: 07/13/1984
• Status: Expired due to Fees

• Current Assignee: Tonachel; Pierre A.
• Original Assignee: Tonachel; Pierre A.
• Inventors: Chang, Robert P.
• Primary Examiner(s): Alvo, Steve
• Application Number:
  US07/460,042
• Time in Patent Office: 196 Days
• Field of Search: 162/19, 162/72, 162/77, 162/76, 127/37, 435/161, 435/163
• US Class Current: 162/19
• CPC Class Codes: C08H 6/00 Macromolecular compounds derived from lignin, e.g. tannins, humic acids
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32
• CPC Class Codes: D21C 3/20 with organic solvents or in solvent environment

Abstract

A method for the continuous countercurrent production of lignins and sugars from wood and other ligno cellulosic materials by organosolv delignification or saccharification at elevated temperatures and pressures is disclosed. The novel method comprises: (a) continuously introducing comminuted lignocellulose materials with a natural mositure content into a reaction vessel from one end; (b) continuously introducing a cooking liquor comprising a major proportion of organic solvent, a minor proportion of water, and a slight amount of inorganic acid countercurrently into the reaction vessel from the opposite end; (c) causing the comminuted lignocellulosic material to be contacted by the cooking liquor; and (d) continuously withdrawing cooking liquor from the reaction vessel after it has commingled with and has dissolved sugars and lignin and other substances from the comminuted lignocellulosic material.

Claims

1. In a method for continuous organosolv treatment of a comminuted lignocellulose material containing naturally occurring water in a reaction vessel, wherein the lignocellulose material is contacted at elevated temperatures with a mixture of an organic solvent, water and a catalytic amount of an acid as a cooking liquor which facilitates the dissolution of the lignocellulose material, the improvement which comprises:

(a) introducing the lignocellulosic material into the vessel through a first inlet in countercurrent flow to the cooking liquor such that in a first zone of the vessel mainly lignin and hemicellulosic sugars are dissolved from the lignocellulosic material leaving a remaining cellulose and such that in a second zone of the vessel spaced from the first zone mainly oligomeric sugars are formed from the remaining cellulose;

(b) introducing the cooking liquor through a second inlet into the second zone in the vessel in countercurrent flow to the lignocellulosic material at a first temperature T₁ in the vessel and removing the cooling liquor in the first zone from a first outlet from the vessel at a temperature T₂ lower than T₁, wherein the water in the comminuted lignocellulosic material introduced into the first zone dilutes the cooking liquor and provides the temperature T₁ for dissolution of the lignin and hemicelluloses in the first zone which are removed from the first zone through the first outlet; and

(c) rapidly cooling the cooking liquor after removing the cooking liquor from the vessel wherein the lignin remains dissolved in the cooking liquor during the cooling.

2. The method of claim 1 wherein a portion of the cooking liquor is removed from an intermediate outlet of the vessel between the first and second zones such that essentially oligomeric sugars are removed through the intermediate outlet and then are rapidly cooled.

3. The method of claim 2 wherein in addition cooking liquor is introduced through an intermediate inlet between the first and second zones and wherein the intermediate inlet is closer to the first zone than the intermediate outlet.

4. The method of claim 3 wherein the cooking liquor introduced into the intermediate inlet has a different organic solvent to water ratio or temperature than the cooking liquor introduced to the first inlet to the vessel such that removal of the hemiculluloses and lignin in the first zone is facilitated.

5. The method of claim 1 wherein additional intermediate inlets, outlets or combinations thereof are provided between the first and second zones.

6. The method of claim 1 wherein the lignocellulosic material is wood containing between 30 and 70 weight percent naturally occurring water.

7. A method of dissolving lignin and sugar substances from comminuted lignocellulosic material at elevated temperatures and pressures comprising:

(a) introducing comminuted lignocellulosic material into a reaction vessel;

(b) introducing a cooking liquor comprising a major proportion of organic solvent, a minor proportion of water, and a catalytically effective amount of inorganic acid into the reaction vessel;

(c) causing the comminuted lignocellulosic material to be contacted by and dissolved in the cooking liquor wherein the flow of cooking liquor is countercurrent to the flow of lignocellulosic material;

(d) withdrawing cooking liquor from the reaction vessel after the liquor has hydrolyzed and dissolved a substantial amount of the sugars, lignin and other substances in the comminuted lignocellulosic material; and

(e) rapidly cooling the cooking liquor wherein the lignin remains dissolved in the cooking liquor during the cooling.

8. A method according to claim 7 wherein the method is conducted at temperatures ranging from 150°

C. to 210°

C.

9. A method according to claim 7 wherein the proportion of organic solvent in the cooking liquor introduced into the reaction vessel is 70 to 90 percent by volume of the cooking liquor.

10. A method according to claim 7 wherein the proportion of organic solvent in the cooking liquor introduced into the reaction vessel is about 80 percent by volume of the cooking liquor.

11. A method according to claim 7 wherein the water content of the comminuted lignocellulose material introduced into the reaction vessel is in the range 30 to 70 percent by weight of the comminuted cellulose material, and wherein the water content of the lignocellulosic material decreases as the material moves through the reactor.

12. A method according to claim 7 wherein the temperature of the cooking liquor introduced into the reaction vessel is about 200°

C. which is maintained at a second zone of the reactor and decreases to 180°

C. at a first zone of the reactor.

13. A method according to claim 7 wherein the time during which the comminuted lignocellulosic material is in contact with the cooking liquor is in the range of about 2 to about 5 minutes.

14. A method according to claim 7 wherein the ratio by weight of cooking liquor to comminuted lignocellulosic material introduced into the reaction vessel is in the range 5:

1 to 15;

1.