WO2023147250A1 - Methanol explosion of cellulosic fibers - Google Patents
Methanol explosion of cellulosic fibers Download PDFInfo
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- WO2023147250A1 WO2023147250A1 PCT/US2023/060905 US2023060905W WO2023147250A1 WO 2023147250 A1 WO2023147250 A1 WO 2023147250A1 US 2023060905 W US2023060905 W US 2023060905W WO 2023147250 A1 WO2023147250 A1 WO 2023147250A1
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- operationally connected
- liquid
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- pressure
- tank
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Links
- 238000004880 explosion Methods 0.000 title claims abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims description 39
- 239000000835 fiber Substances 0.000 title description 13
- 238000000622 liquid--liquid extraction Methods 0.000 claims abstract description 16
- 238000000638 solvent extraction Methods 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 229930013686 lignan Natural products 0.000 claims abstract 11
- 150000005692 lignans Chemical class 0.000 claims abstract 11
- 235000009408 lignans Nutrition 0.000 claims abstract 11
- 229920005610 lignin Polymers 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 19
- 239000003960 organic solvent Substances 0.000 claims description 11
- 239000002028 Biomass Substances 0.000 claims description 9
- 229920002488 Hemicellulose Polymers 0.000 claims description 8
- 235000000346 sugar Nutrition 0.000 claims description 8
- 150000008163 sugars Chemical class 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims 1
- 239000002904 solvent Substances 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000012691 depolymerization reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000012620 biological material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
Definitions
- This disclosure relates generally to chemical engineering, and, more specifically, to a method and apparatus for using organic solvents, such as methanol, to explosively separate clean, free, and depolymerized lignin from cellulosic materials and the harvesting of both.
- organic solvents such as methanol
- Lignin is the most abundant natural aromatic polymer. Lignin has a high storage capacity for phenolic compounds, and as such is a potential source for polymers and biomaterials. However, access to those polymers and biomaterials is difficult, as lignin is both complex and not very reactive.
- FIG. 1 is a process flowsheet for production of clean depolymerized lignin and clean cellulose from biomass.
- the present novel technology relates to a process for the explosive separation of lignin from cellulosic material using an organic solvent, such as methanol; the depolymerization of the so-separated lignin; and the extraction of clean lignin from the depolymerization yield.
- an organic solvent such as methanol
- a quantity of biomass feedstock such as wood chips and/or rice straw, are placed in a tank and soaked in an organic solvent.
- the feedstock is soaked in methanol, as methanol has a relatively low boiling point (as compared to water).
- the fibers may be soaked for a predetermined amount of time at room temperature, or at some elevated temperature below the solvent boiling point to speed the kinetics of the soaking process.
- the soaked fibers are then moved to a high-pressure tank and additional solvent is added, wherein the pressure is increased and the mixture is superheated; the increased pressure is sufficiently great such that the solvent remains in liquid form when superheated.
- the additional solvent is preheated before introduction into the high-pressure tank.
- the novel process enjoys the advantages of not requiring the removal of water for downstream processing.
- the organic solvent may be chosen for being more effective in swelling natural fibers (like, for example, methanol).
- the organic solvent may be selected for having a boiling point lower than that of water, so that similar pressures that drive the explosion process can be achieved at lower temperatures with lower associated energy costs.
- the separated lignin is depolymerized.
- the vapor-exploded fibers with solvent are placed in a high-pressure reactor vessel, which may or may not be the same vessel as the vapor explosion unit described above. Additional ingredients such as catalysts (such as nickel or the like), hydrogen, nitrogen, and/or acid are added to the reactor, which is then heated to temperatures that are super-critical and thus generate high pressures, typically between 20 bars and 300 bars. The super-critical conditions with their attendant high temperatures increase the rate of the lignin depolymerization reaction.
- Methanol is the solvent used in the current example. Methanol is attractive because it is readily available, readily swells the fibers, has a low boiling compared to other alcohols but remains a liquid with a relatively low vapor pressure, and is one of the components in the composite board resin system that has been developed using the depolymerized lignin, thereby alleviating the need to fully remove the methanol.
- other solvents such as ethanol, isopropyl alcohol, mixtures of the above-listed alcohols, and the like, may also be useful, where the associated process would be similar with different temperatures and pressures required for both the vapor-explosion and lignin depolymerization reaction.
- the depolymerization reaction is most commonly done using a metal catalyst, such as supported nickel.
- lignin depolymerization may also be achieved at super-critical temperatures using just high-pressure hydrogen without any metal catalyst. This removes the cost of catalyst preparation as well as the cost of recovery of the catalyst from the reaction products.
- a filter press or the like is used to separate the lignin-free fibers from the solvent phase containing the depolymerized lignin. Any remaining solvent in the fibers is removed by drying, where the solvent is then recaptured and returned to the process.
- the liquid phase from the filter press is then put into a flash evaporator and/or a distillation unit to remove some, but not necessarily all, of the solvent thereby concentrating the depolymerized lignin and any other components in the liquid phase. Solvent may be recovered and recycled back to the process.
- the resulting brown liquor contains the depolymerized lignin as well as other components, such as sugars, hemi-cellulose, small amounts of small cellulose fibers that made it past the filter press, some silica and other inorganic material, and the like. Any remaining cellulose fibers and inorganic particulates like silica may be removed in a settling tank or by mild centrifugation.
- the above methodology may be applied to a variety of agricultural and forestry sources of biomass, including wheat straw, corn stover, sugar cane bagasse, and the like.
- biomass include wheat straw, corn stover, sugar cane bagasse, and the like.
- the only real requirement is that the biomass have a significant amount of lignin.
- aqueous salt solution with sufficient molarity forms a two-phase mixture at room temperature with organic solvents (such as, in this case 1 M NaCI in methanol at room temperature to yield a two-phase mixture).
- organic solvents such as, in this case 1 M NaCI in methanol at room temperature to yield a two-phase mixture.
- the sugars and hemi-cellulose are primarily in the aqueous phase, while the depolymerized lignin remains primarily in the organic phase.
- liquid-liquid extraction be employed to separate the sugars and hemi-cellulose from the brown liquor, resulting in clean depolymerized lignin.
- the sugars and hemi-cellulose are then separated from the salt solution using membrane technology, where the aqueous salt solution is then recycled to the process.
- the sugars and hemi-cellulose are a product of the process in addition to the clean depolymerized lignin and the clean cellulose fibers.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
A lignan separation and depolymerization assembly, including a soaking tank, an intake port operationally connected to the soaking tank, a high-pressure vapor explosion tank connected in fluidic communication with the soaking tank, and a knockout tank connected in fluidic communication with the high-pressure vapor explosion tank. The assembly further includes a high-pressure reactor vessel operationally connected to the high-pressure vapor explosion tank, at least one input port operationally connected to the high-pressure vessel, a filter press operationally connected to the high-pressure reactor vessel, a flash separator operationally connected to the filter press, a settling vessel operationally connected to the flash separator, and a dryer operationally connected to the filter press. The assembly also includes a liquid-liquid extraction vessel having an outlet port, an inlet port, and wherein the liquid-liquid extraction vessel is operationally connected to the settling vessel and a membrane separator operationally connected to the liquid-liquid extraction vessel, wherein the membrane separator both receives material from the liquid-liquid extraction vessel and supplies material to the liquid-liquid extraction vessel.
Description
METHANOL EXPLOSION OF CELLULOSIC FIBERS
CROSS-REFERENCE TO RELATED APPLICATIONS
This patent application claims priority to co-pending U.S. Provisional Patent Application Serial No. 63/304724, filed 31 January 2022.
TECHNICAL FIELD
[0001] This disclosure relates generally to chemical engineering, and, more specifically, to a method and apparatus for using organic solvents, such as methanol, to explosively separate clean, free, and depolymerized lignin from cellulosic materials and the harvesting of both.
BACKGROUND
[0002] This section introduces aspects that may help facilitate a better understanding of the disclosure. Accordingly, these statements are to be read in this light and are not to be understood as admissions about what is or is not prior art.
[0003] Lignin is the most abundant natural aromatic polymer. Lignin has a high storage capacity for phenolic compounds, and as such is a potential source for polymers and
biomaterials. However, access to those polymers and biomaterials is difficult, as lignin is both complex and not very reactive.
[0004] One method of accessing the locked-in polymers and biomaterials is through depolymerization of the lignin. Steam has been used to explosively separate lignin from biomass fibers. Steam separation is advantageous because water is cheap and plentiful. However, steam explosion of biomass requires a fairly great amount of heat and also requires a nickel catalyst, which poses an initial expense as well as a back-end removal expense. Thus, there is a need for a lignin/cellulosic material separation process that requires less heat input and can be performed without the need of a catalyst. The present novel technology addresses this need.
BRIEF DESCRIPTION OF THE DRAWINGS
[0005] FIG. 1 is a process flowsheet for production of clean depolymerized lignin and clean cellulose from biomass.
DETAILED DESCRIPTION
[0006] For the purposes of promoting an understanding of the principles of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the disclosure is thereby intended.
[0007] The present novel technology relates to a process for the explosive separation of lignin from cellulosic material using an organic solvent, such as methanol; the depolymerization of the so-separated lignin; and the extraction of clean lignin from the depolymerization yield.
[0008] First, a quantity of biomass feedstock, such as wood chips and/or rice straw, are placed in a tank and soaked in an organic solvent. In this example, the feedstock is soaked in methanol, as methanol has a relatively low boiling point (as compared to water). The fibers may be soaked for a predetermined amount of time at room temperature, or at some elevated temperature below the solvent boiling point to speed the kinetics of the soaking process.
[0009] The soaked fibers are then moved to a high-pressure tank and additional solvent is added, wherein the pressure is increased and the mixture is superheated; the increased pressure is sufficiently great such that the solvent remains in liquid form when
superheated. In some embodiments, the additional solvent is preheated before introduction into the high-pressure tank.
[0010] The pressure within the tank is then rapidly reduced, such that the solvent rapidly boils. The solvent soaked within the now-swelled fibers rapidly boils and explodes the fibers. The escaping evolved solvent vapor is collected in a knockout tank fluidically connected to the high-pressure tank, condensed back into a liquid state, and recycled for reuse.
[0011] While the process has similarities to known methods of steam explosion of fibers, the novel process enjoys the advantages of not requiring the removal of water for downstream processing. Further, the organic solvent may be chosen for being more effective in swelling natural fibers (like, for example, methanol). Also, the organic solvent may be selected for having a boiling point lower than that of water, so that similar pressures that drive the explosion process can be achieved at lower temperatures with lower associated energy costs.
[0012] Next, the separated lignin is depolymerized. The vapor-exploded fibers with solvent are placed in a high-pressure reactor vessel, which may or may not be the same vessel as the vapor explosion unit described above. Additional ingredients such as catalysts (such as nickel or the like), hydrogen, nitrogen, and/or acid are added to the reactor, which is then heated to temperatures that are super-critical and thus generate high pressures, typically between 20 bars and 300 bars. The super-critical conditions
with their attendant high temperatures increase the rate of the lignin depolymerization reaction.
[0013] Methanol is the solvent used in the current example. Methanol is attractive because it is readily available, readily swells the fibers, has a low boiling compared to other alcohols but remains a liquid with a relatively low vapor pressure, and is one of the components in the composite board resin system that has been developed using the depolymerized lignin, thereby alleviating the need to fully remove the methanol. However, other solvents such as ethanol, isopropyl alcohol, mixtures of the above-listed alcohols, and the like, may also be useful, where the associated process would be similar with different temperatures and pressures required for both the vapor-explosion and lignin depolymerization reaction.
[0014] The depolymerization reaction is most commonly done using a metal catalyst, such as supported nickel. However, lignin depolymerization may also be achieved at super-critical temperatures using just high-pressure hydrogen without any metal catalyst. This removes the cost of catalyst preparation as well as the cost of recovery of the catalyst from the reaction products.
[0015] Once the lignin depolymerization reaction is complete, a filter press or the like is used to separate the lignin-free fibers from the solvent phase containing the depolymerized lignin. Any remaining solvent in the fibers is removed by drying, where the solvent is then recaptured and returned to the process. The liquid phase from the filter press is then put into a flash evaporator and/or a distillation unit to remove some, but not necessarily all, of the solvent thereby concentrating the depolymerized lignin and
any other components in the liquid phase. Solvent may be recovered and recycled back to the process.
[0016] The resulting brown liquor contains the depolymerized lignin as well as other components, such as sugars, hemi-cellulose, small amounts of small cellulose fibers that made it past the filter press, some silica and other inorganic material, and the like. Any remaining cellulose fibers and inorganic particulates like silica may be removed in a settling tank or by mild centrifugation.
[0017] The above methodology may be applied to a variety of agricultural and forestry sources of biomass, including wheat straw, corn stover, sugar cane bagasse, and the like. The only real requirement is that the biomass have a significant amount of lignin.
[0018] It is generally desirable to remove the hemi-cellulose and sugars from the brown liquor. An aqueous salt solution with sufficient molarity forms a two-phase mixture at room temperature with organic solvents (such as, in this case 1 M NaCI in methanol at room temperature to yield a two-phase mixture). The sugars and hemi-cellulose are primarily in the aqueous phase, while the depolymerized lignin remains primarily in the organic phase. Thus, liquid-liquid extraction be employed to separate the sugars and hemi-cellulose from the brown liquor, resulting in clean depolymerized lignin.
[0019] The sugars and hemi-cellulose are then separated from the salt solution using membrane technology, where the aqueous salt solution is then recycled to the process. The sugars and hemi-cellulose are a product of the process in addition to the clean depolymerized lignin and the clean cellulose fibers.
[0020] While the novel technology has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character. It is understood that the embodiments have been shown and described in the foregoing specification in satisfaction of the best mode and enablement requirements. It is understood that one of ordinary skill in the art could readily make a nigh-infinite number of insubstantial changes and modifications to the above-described embodiments and that it would be impractical to attempt to describe all such embodiment variations in the present specification. Accordingly, it is understood that all changes and modifications that come within the spirit of the novel technology are desired to be protected.
Claims
1. A lignan separation and depolymerization apparatus, comprising: a first modular portion, further comprising: a soaking tank; an intake port operationally connected to the soaking tank; a high-pressure vapor explosion tank connected in fluidic communication with the soaking tank; and a knockout tank connected in fluidic communication with the high-pressure vapor explosion tank; a second modular portion operationally connected to the first modular portion, further comprising: a high-pressure reactor vessel; at least one input port operationally connected to the high-pressure vessel; a filter press operationally connected to the high-pressure reactor vessel; a flash separator operationally connected to the filter press; a settling vessel operationally connected to the flash separator; and a dryer operationally connected to the filter press; and a third modular portion operationally connected to the second modular portion, further comprising: a liquid-liquid extraction vessel having an outlet port and an inlet port;
a membrane separator operationally connected to the liquid-liquid extraction vessel, wherein the membrane separator both receives material from the liquid-liquid extraction vessel and supplies material to the liquid-liquid extraction vessel.
2. The lignan separation and depolymerization apparatus of claim 1 wherein the liquid-liquid extraction vessel is operationally connected to the settling vessel; and wherein the high-pressure reactor vessel is operationally connected to the high-pressure vapor explosion tank.
3. The lignan separation and depolymerization apparatus of claim 1 wherein and organic solvent fills the soaking tank.
4. The lignan separation and depolymerization apparatus of claim 3 wherein the organic solvent has a boiling point below 100 degrees Celsius at atmospheric pressure.
5. The lignan separation and depolymerization apparatus of claim 4 wherein the organic solvent is methanol.
6. The lignan separation and depolymerization apparatus of claim 1 wherein the settling vessel is a centrifuge.
A lignan separation and depolymerization assembly, comprising: a soaking tank; an intake port operationally connected to the soaking tank; a high-pressure vapor explosion tank connected in fluidic communication with the soaking tank; and a knockout tank connected in fluidic communication with the high-pressure vapor explosion tank; a high-pressure reactor vessel operationally connected to the high-pressure vapor explosion tank; at least one input port operationally connected to the high-pressure vessel; a filter press operationally connected to the high-pressure reactor vessel; a flash separator operationally connected to the filter press; a settling vessel operationally connected to the flash separator; and a dryer operationally connected to the filter press; and a liquid-liquid extraction vessel having an outlet port, an inlet port, and wherein the liquid-liquid extraction vessel is operationally connected to the settling vessel; and a membrane separator operationally connected to the liquid-liquid extraction vessel, wherein the membrane separator both receives material from the liquid-liquid extraction vessel and supplies material to the liquid-liquid extraction vessel.
8. The lignan separation and depolymerization assembly wherein the soaking tank is filled with methanol.
9. A method of recovering lignan from biomass, comprising: a) soaking a quantity of biomass in an organic solvent to yield a first product; b) superheating the first product under elevated pressure; c) rapidly reducing the pressure on the superheated first product; d) explosively separating lignin from residual cellulosic material to yield separated lignin and residual cellulosic material; e) depolymerizing the separated lignin; and f) segregating the depolymerized lignin.
10. The method of recovering lignan from biomass of claim 9 and further comprising: g) after d) and before e), capturing evolved organic solvent for reuse.
11. The method of claim 9 wherein step e) further comprises exposing the separated lignin to a catalyst-free hydrogen environment under elevated temperature and pressure.
12. The method of claim 9 wherein step f) further comprises separating depolymerized lignin from sugars and hemi-cellulose, and wherein the sugars and hemicellulose are harvested for later use.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US202263304724P | 2022-01-31 | 2022-01-31 | |
| US63/304,724 | 2022-01-31 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2023147250A1 true WO2023147250A1 (en) | 2023-08-03 |
Family
ID=87472477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2023/060905 WO2023147250A1 (en) | 2022-01-31 | 2023-01-19 | Methanol explosion of cellulosic fibers |
Country Status (1)
| Country | Link |
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| WO (1) | WO2023147250A1 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4966650A (en) * | 1987-09-17 | 1990-10-30 | Delong Edward A | Method for fractionation of lignins from steam exploded lignocellulosics to provide fractions with different properties |
| US20100041119A1 (en) * | 2005-07-19 | 2010-02-18 | Holm Christensen Biosystemer Aps | Method and apparatus for conversion of cellulosic material to ethanol |
| US20100135843A1 (en) * | 2007-03-08 | 2010-06-03 | Torjorn Van Der Van Der Meulen | Apparatus for extraction of saccharides from lignocellulose material by means of hydrolysis and use of a certain material in the apparatus |
| US20150329889A1 (en) * | 2012-12-18 | 2015-11-19 | Stichting Energieonderzoek Centrum Nederland | Process for enzymatic hydrolysis of cellulose |
| US20180216141A1 (en) * | 2015-03-26 | 2018-08-02 | The Texas A & M University System | Invention CONVERSION OF LIGNIN INTO BIOPLASTICS AND LIPID FUELS |
-
2023
- 2023-01-19 WO PCT/US2023/060905 patent/WO2023147250A1/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4966650A (en) * | 1987-09-17 | 1990-10-30 | Delong Edward A | Method for fractionation of lignins from steam exploded lignocellulosics to provide fractions with different properties |
| US20100041119A1 (en) * | 2005-07-19 | 2010-02-18 | Holm Christensen Biosystemer Aps | Method and apparatus for conversion of cellulosic material to ethanol |
| US20100135843A1 (en) * | 2007-03-08 | 2010-06-03 | Torjorn Van Der Van Der Meulen | Apparatus for extraction of saccharides from lignocellulose material by means of hydrolysis and use of a certain material in the apparatus |
| US20150329889A1 (en) * | 2012-12-18 | 2015-11-19 | Stichting Energieonderzoek Centrum Nederland | Process for enzymatic hydrolysis of cellulose |
| US20180216141A1 (en) * | 2015-03-26 | 2018-08-02 | The Texas A & M University System | Invention CONVERSION OF LIGNIN INTO BIOPLASTICS AND LIPID FUELS |
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