CN115976866A - Method for separating components of lignocellulose biomass by pretreatment of lignocellulose with organic solvent - Google Patents
Method for separating components of lignocellulose biomass by pretreatment of lignocellulose with organic solvent Download PDFInfo
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- CN115976866A CN115976866A CN202211467403.8A CN202211467403A CN115976866A CN 115976866 A CN115976866 A CN 115976866A CN 202211467403 A CN202211467403 A CN 202211467403A CN 115976866 A CN115976866 A CN 115976866A
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- lignin
- triethylene glycol
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- hemicellulose
- filter residue
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002028 Biomass Substances 0.000 title claims abstract description 20
- 239000003960 organic solvent Substances 0.000 title claims abstract description 8
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229920005610 lignin Polymers 0.000 claims abstract description 44
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 35
- 229920002678 cellulose Polymers 0.000 claims abstract description 34
- 239000001913 cellulose Substances 0.000 claims abstract description 34
- 239000000706 filtrate Substances 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 5
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 4
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920001221 xylan Polymers 0.000 claims abstract description 4
- 150000004823 xylans Chemical class 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 11
- 239000002029 lignocellulosic biomass Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000002154 agricultural waste Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000012296 anti-solvent Substances 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 15
- 238000000605 extraction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 44
- 230000000052 comparative effect Effects 0.000 description 14
- 102000004190 Enzymes Human genes 0.000 description 6
- 108090000790 Enzymes Proteins 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 241000609240 Ambelania acida Species 0.000 description 5
- 239000010905 bagasse Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical group O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 244000062720 Pennisetum compressum Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for separating components of lignocellulose biomass by organic solvent pretreatment. The method comprises the following steps: adding lignocellulose biomass and a triethylene glycol solution into a reaction vessel for reaction, then carrying out solid-liquid separation on the triethylene glycol solution containing an acidic catalyst to obtain filter residue containing cellulose components and a filtrate dissolved with hemicellulose and lignin; adding a reverse solvent into the filtrate, and performing solid-liquid separation to obtain filter residue containing lignin and hemicellulose components and filtrate; adding filter residue containing lignin and hemicellulose components into a hydrochloric acid solution, stirring, and performing solid-liquid separation to obtain lignin component residue and filtrate containing xylose and xylan. The method provided by the invention is used for resolving and dissolving out the raw materials of lignin and hemicellulose in an acidic triethylene glycol system, and recovering the lignin and the hemicellulose in the solution step by step, so that the separation and extraction of each component in the lignocellulose biomass are realized.
Description
The technical field is as follows:
the invention relates to the technical field of biomass energy conversion and utilization, in particular to a method for separating components of lignocellulose biomass by pretreatment of an organic solvent.
Background art:
lignocellulosic biomass is a recognized renewable resource that can be converted to fuels, materials, and chemicals by biorefinery processes. However, cellulose, hemicellulose and lignin components forming the lignocellulose biomass are mutually connected to form a compact and complex three-dimensional space structure, and the components are difficult to be effectively and directly converted and utilized, so that the components are often separated by a pretreatment means, so that the subsequent conversion and utilization of the components are facilitated, the utilization efficiency of the three major components of the biomass is improved, and the biorefinery process of the lignocellulose biomass is further realized.
In recent years, organic solvent pretreatment is one of the main methods for achieving separation of components of lignocellulosic biomass. Patent CN106674538A discloses a method for separating and extracting cellulose, hemicellulose degraded sugar and lignin from bamboo wood, and provides a lignocellulose component separation process with gamma-valerolactone aqueous solution as a solvent under the action of acid; patent ZL201510813243.1 discloses a green process for separating lignocellulose components, which realizes the separation of the lignocellulose components by irradiating pretreated biomass and coupling tetrahydrofuran or gamma-valerolactone reaction; patent ZL201410006095.8 discloses a method for preparing cellulose and lignin under the assistance of normal pressure ultrasonic waves by taking high-boiling alcohol as a solvent, wherein the cellulose and the lignin in biomass are separated by cooking in a high-boiling alcohol solution at 130-140 ℃; patent ZL202010101379.0 discloses a method for efficiently separating lignocellulose and performing enzymolysis through an ionic liquid-high-boiling-point alcohol composite system, and the separation efficiency of components of biomass is further improved through a multi-step composite pretreatment mode. Although the lignocellulose structure can be effectively broken through the method for separating the organic solvent components, and partial or complete separation of the components can be realized, the efficient component separation technology usually needs higher reaction temperature (> 150 ℃), the multi-step pretreatment method brings complex process steps such as solvent circulation and hemicellulose and lignin separation, and the problems of high energy consumption and high environmental pressure are easily generated in the practical application process.
The invention content is as follows:
the invention solves the problems in the prior art, and provides a method for separating components of lignocellulose biomass by organic solution pretreatment.
The invention aims to provide a method for separating components of lignocellulose biomass by organic solvent pretreatment, which comprises the following steps: adding lignocellulose biomass and a triethylene glycol solution into a reaction container, reacting the triethylene glycol solution containing an acid catalyst at 80-140 ℃ for 0.1-6 h, and performing solid-liquid separation to obtain filter residue containing cellulose components and filtrate dissolved with hemicellulose and lignin; adding a reverse solvent into the filtrate, carrying out solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, carrying out reduced pressure distillation on the filtrate, and recovering the reverse solvent and a triethylene glycol solution; adding the filter residue containing the lignin and hemicellulose components into a hydrochloric acid solution, stirring, and carrying out solid-liquid separation to obtain lignin component residue and filtrate containing xylose and xylan.
Preferably, the mass-to-volume ratio of the lignocellulosic biomass to the triethylene glycol solution is 1: (8-20) g/mL.
Preferably, the volume fraction of the triethylene glycol in the triethylene glycol solution is 50-100%, and the concentration of the acid catalyst is 0.05-0.20 mol/L.
Preferably, the acidic catalyst is soluble acid or strong acid and weak base salt, the acid is selected from one of sulfuric acid, hydrochloric acid, formic acid and methyl benzene sulfonic acid, and the strong acid and weak base salt is selected from one of ferric sulfate, aluminum trichloride and copper nitrate.
Preferably, 8 times the volume of the filtrate of the counter solvent is added to the filtrate, and the counter solvent is diethyl ether.
Preferably, the mass volume ratio of the filter residue containing the lignin and the hemicellulose components to the hydrochloric acid solution is 1:10g/mL, the mass concentration of the hydrochloric acid solution is 1%.
Preferably, the particle size of the lignocellulosic biomass is 0.5 to 3mm.
Preferably, the lignocellulosic biomass is an energy plant or waste containing at least cellulose and lignin. The energy plant comprises pennisetum alopecuroides and the like.
Further preferably, the waste is forestry waste, agricultural waste or processing waste. Forestry waste comprises wood chips and the like, agricultural waste comprises straws and the like, and processing waste is sugar mill or brewery processing waste comprising bagasse, furfural residues and the like.
Compared with the prior art, the invention has the following advantages:
(1) The method utilizes the excellent lignin dissolving capacity of the acidic triethylene glycol to separate the lignocellulose biomass under mild conditions, so that the cellulose component and the lignin component which are raw materials are separated and recovered in the form of filter residues, and the hemicellulose component is separated and recovered in the form of dissolved xylose and xylan.
(2) The cellulose component content of the filter residue rich in the cellulose component is high, and the filter residue is easy to carry out enzymolysis, conversion and utilization.
(3) The high-boiling-point triethylene glycol has good biocompatibility and low pressure in the reaction process.
(4) The invention has wide raw material application range, can recycle the used solvent and can effectively reduce the cost.
The specific implementation mode is as follows:
the following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention. Unless otherwise specified, the experimental materials and reagents used herein are all conventional commercial products in the art.
Example 1
Taking 2g of bagasse (containing 40.1% of cellulose, 24.3% of hemicellulose and 18.2% of lignin) with the particle size of 0.5mm as a raw material, and mixing the raw material and a triethylene glycol solution according to the mass volume ratio of 1: adding a triethylene glycol solution with sulfuric acid concentration of 0.2mol/L and triethylene glycol volume fraction of 100% into the reactor by 8 g/mL; after the reaction is carried out for 0.5h at the temperature of 100 ℃, carrying out solid-liquid separation to obtain 1.02g of filter residue with the cellulose content of 71.8% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose is used for enzymolysis for 72h at the temperature of 50 ℃, and the enzymolysis rate is 80.1%); adding 8 times of filtrate volume of diethyl ether into the filtrate, performing solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, distilling the filtrate under reduced pressure, and recovering diethyl ether and triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
Comparative example 1
Comparative example 1 was conducted in the same manner as in example 1 except that ethylene glycol was used instead of triethylene glycol used in example 1.
Comparative example 2
Comparative example 2 was conducted in the same manner as in example 1 except that polyethylene glycol 400 was used in place of the triethylene glycol used in example 1.
Comparative example 3
Comparative example 3 was conducted as in example 1 except that ethanol was used instead of the triethylene glycol used in example 1.
Comparative example 4
Comparative example 4 was conducted in the same manner as in example 1 except that glycerin was used instead of triethylene glycol used in example 1.
The filter residue and lignin recovery amounts of example 1 and comparative examples 1 to 4 are shown in table 1:
TABLE 1
| Filtering residue | Cellulose content of filter residue | Cellulose enzymolysis rate | |
| Example 1 | 1.02g | 71.8％ | 80.1％ |
| Comparative example 1 | 1.11g | 65.4％ | 63.3％ |
| Comparative example 2 | 1.26g | 60.4％ | 57.7％ |
| Comparative example 3 | 1.15g | 62.1％ | 64.2％ |
| Comparative example 4 | 1.22g | 61.1％ | 52.2％ |
From the above table, it can be seen that the triethylene glycol solution filter residue has the highest cellulose content and the highest cellulose hydrolysis rate, which indicates that the triethylene glycol solution has an obvious advantage in the separation performance of the components of the lignocellulose biomass compared with the comparative alcohol solution.
Example 2
Taking 2g of bagasse (containing 40.1% of cellulose, 24.3% of hemicellulose and 18.2% of lignin) with the particle size of 0.5mm as a raw material, and mixing the raw material and a triethylene glycol solution according to the mass volume ratio of 1: adding a triethylene glycol solution with sulfuric acid concentration of 0.05mol/L and triethylene glycol volume fraction of 50% into the reactor in an amount of 8 g/mL; after reacting for 6h at 80 ℃, carrying out solid-liquid separation to obtain 1.36g of filter residue with the cellulose content of 54.5% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose, enzymolysis is carried out for 72h at 50 ℃, and the enzymolysis rate is 43.3%); adding 8 times of filtrate volume of diethyl ether into the filtrate, performing solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, distilling the filtrate under reduced pressure, and recovering diethyl ether and triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
Example 3
Taking 2g of bagasse (containing 40.1% of cellulose, 24.3% of hemicellulose and 18.2% of lignin) with the particle size of 3.0mm as a raw material, and mixing the raw material and a triethylene glycol solution according to the mass volume ratio of 1: adding a triethylene glycol solution with sulfuric acid concentration of 0.2mol/L and triethylene glycol volume fraction of 100% into a reactor in an amount of 20 g/mL; after reacting for 0.1h at 140 ℃, carrying out solid-liquid separation to obtain 0.78g of filter residue with the cellulose content of 86.9% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose, enzymolysis is carried out for 72h at 50 ℃, and the enzymolysis rate is 88.4%); adding 8 times volume of diethyl ether into the filtrate, performing solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, distilling the filtrate under reduced pressure, and recovering diethyl ether and triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
Example 4
Taking 2g of bagasse (containing 40.1% of cellulose, 24.3% of hemicellulose and 18.2% of lignin) with the particle size of 3.0mm as a raw material, and mixing the raw material and a triethylene glycol solution according to the mass volume ratio of 1: adding a triethylene glycol solution with sulfuric acid concentration of 0.1mol/L and triethylene glycol volume fraction of 100% into a reactor in an amount of 20 g/mL; after 2 hours of reaction at 100 ℃, carrying out solid-liquid separation to obtain 0.83g of filter residue with the cellulose content of 90.5% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose is used for enzymolysis for 72 hours at 50 ℃, and the enzymolysis rate is 91.7%); adding ethyl ether with the volume of 8 times of the filtrate into the filtrate, carrying out solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, carrying out reduced pressure distillation on the filtrate, and recovering a reverse solvent and a triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
Example 5
Taking 2g of furfural residue (containing 36.4% of cellulose, 1.2% of hemicellulose and 34.5% of lignin) with the granularity of 0.5mm as a raw material, and mixing the raw material and a triethylene glycol solution according to the mass volume ratio of 1: adding a triethylene glycol solution with the concentration of hydrochloric acid of 0.1mol/L and the volume fraction of triethylene glycol of 100% into a reactor in an amount of 10 g/mL; after 2h of reaction at 100 ℃, carrying out solid-liquid separation to obtain 0.86g of filter residue with the cellulose content of 79.9% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose, enzymolysis is carried out for 72h at 50 ℃, and the enzymolysis rate is 84.5%); adding ethyl ether with the volume of 8 times of the filtrate into the filtrate, carrying out solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, carrying out reduced pressure distillation on the filtrate, and recovering a reverse solvent and a triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
Example 6
2g of poplar (containing 46.1% of cellulose, 12.7% of hemicellulose and 24.4% of lignin) with the granularity of 0.5mm is taken as a raw material, and the mass volume ratio of the raw material to a triethylene glycol solution is 1: adding a triethylene glycol solution with the concentration of aluminum chloride of 0.1mol/L and the volume fraction of triethylene glycol of 100% into the amount of 10g/mL in a reactor; after 2h of reaction at 100 ℃, carrying out solid-liquid separation to obtain 1.32g of filter residue with the cellulose content of 64.8% (substrate concentration is 5%, CTec2 enzyme with 20FPU/g cellulose, enzymolysis is carried out for 72h at 50 ℃, and the enzymolysis rate is 55.3%); adding 8 times of filtrate volume of diethyl ether into the filtrate, performing solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, distilling the filtrate under reduced pressure, and recovering diethyl ether and triethylene glycol solution; adding filter residue containing lignin and hemicellulose components into a dilute hydrochloric acid solution with the mass concentration of 1%, wherein the mass volume ratio of the filter residue to the dilute hydrochloric acid solution is 1.
The above embodiments are only for the purpose of helping understanding the technical solution of the present invention and the core idea thereof, and it should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (9)
1. A method for separating components of lignocellulose biomass by organic solvent pretreatment is characterized by comprising the following steps: adding lignocellulose biomass and a triethylene glycol solution into a reaction container, reacting the triethylene glycol solution containing an acid catalyst for 0.1-6 h at 80-140 ℃, and performing solid-liquid separation to obtain filter residue containing cellulose components and filtrate dissolved with hemicellulose and lignin; adding a reverse solvent into the filtrate, carrying out solid-liquid separation to obtain filter residue containing lignin and hemicellulose components, carrying out reduced pressure distillation on the filtrate, and recovering the reverse solvent and a triethylene glycol solution; adding the filter residue containing the lignin and hemicellulose components into a hydrochloric acid solution, stirring, and carrying out solid-liquid separation to obtain lignin component residue and filtrate containing xylose and xylan.
2. The method according to claim 1, wherein the mass-to-volume ratio of the lignocellulosic biomass to the triethylene glycol solution is 1: (8-20) g/mL.
3. The method according to claim 1, wherein the triethylene glycol solution has a volume fraction of triethylene glycol of 50% to 100%, and the concentration of the acid catalyst is 0.05mol/L to 0.20mol/L.
4. The method of claim 1 or 3, wherein the acidic catalyst is a soluble acid or a strong and weak base salt, the acid is selected from one of sulfuric acid, hydrochloric acid, formic acid and methyl benzene sulfonic acid, and the strong and weak base salt is selected from one of ferric sulfate, aluminum trichloride and copper nitrate.
5. The method according to claim 1, wherein 8 times the volume of the filtrate of the anti-solvent is added to the filtrate, and the anti-solvent is diethyl ether.
6. The method according to claim 1, wherein the mass-to-volume ratio of the filter residue containing the lignin and hemicellulose components to the hydrochloric acid solution is 1:10g/mL, the mass concentration of the hydrochloric acid solution is 1%.
7. The method of claim 1, wherein the lignocellulosic biomass has a particle size of 0.5 to 3mm.
8. The method of claim 1, wherein the lignocellulosic biomass is an energy plant or waste containing at least cellulose and lignin.
9. The method of claim 8, wherein the waste is forestry waste, agricultural waste or processing waste.
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| WO1997032075A1 (en) * | 1996-02-29 | 1997-09-04 | Burkart, Leonard | Process for the production of lignin and microcellulose |
| US5859236A (en) * | 1996-02-29 | 1999-01-12 | Burkart; Leonard | Process for preparation of lignin and microcellulose |
| CN103597085A (en) * | 2011-06-10 | 2014-02-19 | 先正达参股股份有限公司 | Methods for converting lignocellulosic material to useful products |
| CN109957983A (en) * | 2017-11-08 | 2019-07-02 | 地球循环株式会社 | Cellulose separation method |
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| US4826566A (en) * | 1988-01-11 | 1989-05-02 | Le Tourneau College | Rapid disolution of lignin and other non-carbohydrates from ligno-cellulosic materials impregnated with a reaction product of triethyleneglycol and an organic acid |
| WO1997032075A1 (en) * | 1996-02-29 | 1997-09-04 | Burkart, Leonard | Process for the production of lignin and microcellulose |
| US5859236A (en) * | 1996-02-29 | 1999-01-12 | Burkart; Leonard | Process for preparation of lignin and microcellulose |
| CN103597085A (en) * | 2011-06-10 | 2014-02-19 | 先正达参股股份有限公司 | Methods for converting lignocellulosic material to useful products |
| CN109957983A (en) * | 2017-11-08 | 2019-07-02 | 地球循环株式会社 | Cellulose separation method |
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