CA1201115A - High efficiency organosolv saccharification process - Google Patents
High efficiency organosolv saccharification processInfo
- Publication number
- CA1201115A CA1201115A CA000395820A CA395820A CA1201115A CA 1201115 A CA1201115 A CA 1201115A CA 000395820 A CA000395820 A CA 000395820A CA 395820 A CA395820 A CA 395820A CA 1201115 A CA1201115 A CA 1201115A
- Authority
- CA
- Canada
- Prior art keywords
- sugars
- cellulosic material
- acetone
- liquor
- pressure vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
HIGH EFFICIENCY ORGANOSOLV
SACCHARIFICATION PROCESS
ABSTRACT OF THE DISCLOSURE
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 per cent by volume of acetone and up to virtually anhydrous acetone. The process is performed at elevated reaction temperatures, preferably at 145°C to 230°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 celluslosic 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. Lignin and sugars derived are commercially useful chemical compounds.
SACCHARIFICATION PROCESS
ABSTRACT OF THE DISCLOSURE
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 per cent by volume of acetone and up to virtually anhydrous acetone. The process is performed at elevated reaction temperatures, preferably at 145°C to 230°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 celluslosic 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. Lignin and sugars derived are commercially useful chemical compounds.
Claims (17)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. In a process for the production of carbohydrate hydrolysates as sugars from a comminuted cellulosic material which can contain lignin by treating the material in a pressure vessel with a solvent mixture of acetone and water containing a small amount of an acidic compound at elevated temperatures between about 145°C and 230°C
to form reducing sugars in a liquor, the improvement which comprises:
(a) providing mixtures of acetone and water containing greater than 70 volume percent acetone and the catalytic acidic compound as the solvent mixture in the pressure vessel at the elevated temperatures with the cellulosic material;
(b) repeatedly treating the cellulosic material in the solvent mixture for a limited period of time at the elevated temperatures until the cellulosic material is at least partially dissolved and such that at least 90 percent of the solubilized sugars from the cellulosic material are recovered without degradation to non-sugars in the liquor; and (c) rapidly cooling the liquor as it is removed from the pressure vessel after each treatment, wherein the cellulosic material is treated on a batch or continuous basis in the pressure vessel using successive amounts of the solvent mixture thereby defining successive stages of treatment at the elevated temperatures, wherein less than 50 percent by weight of the cellulosic material is dissolved in each stage of treatment and wherein in each stage the cellulosic material is treated for a limited period of time in the pressure vessel and then the withdrawn liquor is rapidly cooled when removed from the pressure vessel so as to achieve the sugar recovery.
to form reducing sugars in a liquor, the improvement which comprises:
(a) providing mixtures of acetone and water containing greater than 70 volume percent acetone and the catalytic acidic compound as the solvent mixture in the pressure vessel at the elevated temperatures with the cellulosic material;
(b) repeatedly treating the cellulosic material in the solvent mixture for a limited period of time at the elevated temperatures until the cellulosic material is at least partially dissolved and such that at least 90 percent of the solubilized sugars from the cellulosic material are recovered without degradation to non-sugars in the liquor; and (c) rapidly cooling the liquor as it is removed from the pressure vessel after each treatment, wherein the cellulosic material is treated on a batch or continuous basis in the pressure vessel using successive amounts of the solvent mixture thereby defining successive stages of treatment at the elevated temperatures, wherein less than 50 percent by weight of the cellulosic material is dissolved in each stage of treatment and wherein in each stage the cellulosic material is treated for a limited period of time in the pressure vessel and then the withdrawn liquor is rapidly cooled when removed from the pressure vessel so as to achieve the sugar recovery.
2. The process of claim 1 wherein the concentration of acetone in the acetone and water mixture is between 80 to 90 volume percent.
3. The process of claim 2 wherein the acidic compound is sulfuric acidic and the concentration is less than 2 percent per weight of the acetone-water mixture.
4. The process of claim 3 wherein the acidic compound is hydrochloric acid and the concentration is less than 1 percent per weight of the acetone-water mixture.
5. The process of claim 1 wherein the addition the liquor is further hydrolyzed at elevated temperatures and dilute acid solutions to produce essentially monomeric sugars.
6. The process of claim 1 wherein the liquor is subjected to distillation whereby pentoses are volatilized from the liquor.
7. The process of claims 1, 5 or 6 wherein the aqueous solution contains dissolved sugars in excess of 15 percent solids.
8. The process of claim 3 or 4 wherein the concentration of the acid is between 0.10 Normal and 0.001 Mormal with respect to the acetone-water mixture.
9. The process of claim 1 wherein the volatiles in the liquor are distilled at reduced pressures to leave in aqueous solution in which lignin is precipitated and is separated.
10. In a process for the production of carbohydrate hydrolysates as sugars and lignin from comminuted cellulosic material which can contain lignin by treating the material in a pressure vessel with a solvent mixture of acetone and water containing a small amount of an acidic compound at elevated temperatures between about 145°C and 230°C
to solubilize any lignin and to form reducing sugars in a liquor, the improvement which comprises:
(a) providing mixtures of acetone and water containing greater than 70 volume percent acetone and the catalytic acid compound as the solvent mixture in the pressure vessel at the elevated temperatures with the cellulosic material;
(b) repeatedly treating the cellulosic material in the solvent mixture for limited periods of time at the elevated temperatures until the cellulosic material is at least partially dissolved and such that at least 90 percent of the solubilized sugars from the cellulosic material are recovered without degradation to non-sugars wherein the carbohydrates in the cellulosic material are dissolved and hydrolyzed partially or substantially completely;
(c) continuously removing the liquor from the pressure vessel;
(d) rapidly cooling the liquor by controlled flash evaporation of acetone to form a residual aqueous solution after each treatment, wherein the cellulosic material is treated in the pressure vessel using successive amounts of the solvent mixture thereby defining successive stages of treatment at the elevated temperatures, wherein less than 50 percent of the cellulosic material is dissolved in each stage and wherein in each stage the cellulosic material is treated for a limited period of time in the pressure vessel and then the withdrawn liquor is rapidly cooled when removed from the pressure vessel so as to achieve the sugar recovery,
to solubilize any lignin and to form reducing sugars in a liquor, the improvement which comprises:
(a) providing mixtures of acetone and water containing greater than 70 volume percent acetone and the catalytic acid compound as the solvent mixture in the pressure vessel at the elevated temperatures with the cellulosic material;
(b) repeatedly treating the cellulosic material in the solvent mixture for limited periods of time at the elevated temperatures until the cellulosic material is at least partially dissolved and such that at least 90 percent of the solubilized sugars from the cellulosic material are recovered without degradation to non-sugars wherein the carbohydrates in the cellulosic material are dissolved and hydrolyzed partially or substantially completely;
(c) continuously removing the liquor from the pressure vessel;
(d) rapidly cooling the liquor by controlled flash evaporation of acetone to form a residual aqueous solution after each treatment, wherein the cellulosic material is treated in the pressure vessel using successive amounts of the solvent mixture thereby defining successive stages of treatment at the elevated temperatures, wherein less than 50 percent of the cellulosic material is dissolved in each stage and wherein in each stage the cellulosic material is treated for a limited period of time in the pressure vessel and then the withdrawn liquor is rapidly cooled when removed from the pressure vessel so as to achieve the sugar recovery,
11. The process of claim 10 wherein the cellulosic material is lignocellulosic and wherein the volatiles in the liquor are distilled at reduced pressure to leave the residual aqueous solution and precipitated lignin and wherein the residual aqueous solution is neutralized prior to recovering the sugars.
12. The process of claim 10 wherein the concentration of acetone and water is between 80 to 90 percent.
13. The process of claim 10 wherein the pentose sugars are votalized from the residual aqueous solution as acetone complexes to separate them from the hexose sugars.
14. The process of claim 13 wherein the sugar-acetone complexes are each broken by contacting the complexes with aqueous acid at elevated temperature.
15. The process of claim 14 wherein the complexes are continuously treated with aqueous acid at elevated temperature until sugar dehydration products are formed.
16. The method of claim 10 wherein the cellulosic material is treated in a batch or continuous manner and the recovered solvent fractions are worked up separately or in unison.
17. The method of claim 10 wherein hydrolysis of the cellulosic material is stopped at a point where essenti-ally pure crystalline cellulose is recovered as solid residue from the reactor.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AR28884882A AR227462A1 (en) | 1981-03-26 | 1982-03-23 | IMPROVED PROCEDURE FOR THE PRODUCTION OF CARBOHYDRATE HYDROLYSATES FROM CRUSHED CELLULOSIC MATERIAL |
PCT/EP1982/000068 WO1982003409A1 (en) | 1981-03-26 | 1982-03-26 | High efficiency organosolv saccharification process |
AT82900956T ATE23364T1 (en) | 1981-03-26 | 1982-03-26 | VERY EFFECTIVE SUGARING PROCESS USING ORGANIC SOLVENTS. |
EP19820900956 EP0074983B1 (en) | 1981-03-26 | 1982-03-26 | High efficiency organosolv saccharification process |
JP57501134A JPH0785720B2 (en) | 1981-03-26 | 1982-03-26 | High efficiency organosolv saccharification method |
BR8207243A BR8207243A (en) | 1981-03-26 | 1982-03-26 | HIGH EFFICACY ORGANOSOLV PROCESS AND SACARIFICATION |
DE8282900956T DE3274120D1 (en) | 1981-03-26 | 1982-03-26 | High efficiency organosolv saccharification process |
SU823526203A SU1701115A3 (en) | 1982-02-09 | 1982-06-24 | Method of producing sugar from cellulose containing stock |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US248,023 | 1981-03-26 | ||
US06/248,023 US4409032A (en) | 1977-08-31 | 1981-03-26 | Organosolv delignification and saccharification process for lignocellulosic plant materials |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1201115A true CA1201115A (en) | 1986-02-25 |
Family
ID=22937331
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA000395820A Expired CA1201115A (en) | 1981-03-26 | 1982-02-09 | High efficiency organosolv saccharification process |
Country Status (2)
Country | Link |
---|---|
CA (1) | CA1201115A (en) |
ZA (1) | ZA821756B (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008144878A1 (en) * | 2007-05-31 | 2008-12-04 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US8193324B2 (en) | 2007-05-31 | 2012-06-05 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
CN101711263B (en) * | 2007-05-31 | 2012-11-28 | 丽格诺新创有限公司 | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US9708490B2 (en) | 2009-05-28 | 2017-07-18 | Fibria Innovations Inc. | Derivatives of native lignin |
US9840621B2 (en) | 2011-03-24 | 2017-12-12 | Fibria Innovations Inc. | Compositions comprising lignocellulosic biomass and organic solvent |
US9982174B2 (en) | 2010-02-15 | 2018-05-29 | Fibria Innovations Inc. | Binder compositions comprising lignin derivatives |
US10533030B2 (en) | 2010-02-15 | 2020-01-14 | Suzano Canada Inc. | Carbon fibre compositions comprising lignin derivatives |
-
1982
- 1982-02-09 CA CA000395820A patent/CA1201115A/en not_active Expired
- 1982-03-16 ZA ZA821756A patent/ZA821756B/en unknown
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008144878A1 (en) * | 2007-05-31 | 2008-12-04 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US8193324B2 (en) | 2007-05-31 | 2012-06-05 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US8227004B2 (en) | 2007-05-31 | 2012-07-24 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
CN101711263B (en) * | 2007-05-31 | 2012-11-28 | 丽格诺新创有限公司 | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US8528463B2 (en) | 2007-05-31 | 2013-09-10 | Lignol Innovations Ltd. | Modular system for organosolv fractionation of lignocellulosic feedstock |
US8772427B2 (en) | 2008-11-26 | 2014-07-08 | Lignol Innovations Ltd. | Continuous counter-current organosolv processing of lignocellulosic feedstocks |
US9708490B2 (en) | 2009-05-28 | 2017-07-18 | Fibria Innovations Inc. | Derivatives of native lignin |
US10435562B2 (en) | 2009-05-28 | 2019-10-08 | Fibria Innovations Inc. | Derivatives of native lignin, lignin-wax compositions, their preparation, and uses thereof |
US9982174B2 (en) | 2010-02-15 | 2018-05-29 | Fibria Innovations Inc. | Binder compositions comprising lignin derivatives |
US10533030B2 (en) | 2010-02-15 | 2020-01-14 | Suzano Canada Inc. | Carbon fibre compositions comprising lignin derivatives |
US9840621B2 (en) | 2011-03-24 | 2017-12-12 | Fibria Innovations Inc. | Compositions comprising lignocellulosic biomass and organic solvent |
Also Published As
Publication number | Publication date |
---|---|
ZA821756B (en) | 1983-02-23 |
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