CN115976866B - Method for separating lignocellulose biomass components through pretreatment of organic solvent - Google Patents
Method for separating lignocellulose biomass components through pretreatment of organic solvent Download PDFInfo
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- triethylene glycol
- lignin
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- 239000002028 Biomass Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 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 51
- 229920005610 lignin Polymers 0.000 claims abstract description 50
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 40
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 239000001913 cellulose Substances 0.000 claims abstract description 36
- 229920002678 cellulose Polymers 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000706 filtrate Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 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 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000012296 anti-solvent Substances 0.000 claims abstract description 10
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 9
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 229920001221 xylan Polymers 0.000 claims abstract description 9
- 150000004823 xylans Chemical class 0.000 claims abstract description 9
- 239000003377 acid catalyst Substances 0.000 claims abstract description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 36
- 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
- 239000002253 acid Substances 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 8
- 150000001447 alkali salts Chemical class 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000002029 lignocellulosic biomass Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 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
- 239000002245 particle Substances 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
- 239000002994 raw material Substances 0.000 abstract description 16
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- 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
- 238000009835 boiling Methods 0.000 description 4
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical group O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 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
- 238000011084 recovery Methods 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
- 241000209046 Pennisetum 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
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 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
- 230000000593 degrading effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption 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
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 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
- 239000002023 wood Substances 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 lignocellulose biomass components by pretreatment of an organic solvent. The method comprises the following steps: adding lignocellulose biomass and triethylene glycol solution into a reaction container for reaction, wherein the triethylene glycol solution is the triethylene glycol solution containing an acid catalyst, and carrying out solid-liquid separation to obtain filter residues containing cellulose components and filtrate containing hemicellulose and lignin; adding an anti-solvent into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components and filtrate; adding the filter residue containing lignin and hemicellulose components into hydrochloric acid solution, stirring, and performing solid-liquid separation to obtain lignin component residues and filtrate containing xylose and xylan. According to the invention, raw materials lignin and hemicellulose are disassembled and dissolved in an acidic triethylene glycol system, residual cellulose solids are recovered step by step in a solution, and separation and extraction of each component in lignocellulose biomass are realized.
Description
Technical field:
The invention relates to the technical field of biomass energy conversion and utilization, in particular to a method for separating components of lignocellulose biomass pretreated by an organic solvent.
The background technology is as follows:
Lignocellulosic biomass is a well-known renewable resource that can be converted into fuels, materials, and chemicals by biorefinery. However, the cellulose, hemicellulose and lignin components forming the lignocellulose biomass are mutually connected to form a compact and complex space three-dimensional structure, and each component is difficult to effectively and directly convert and utilize, so that the components are often required to be separated by a pretreatment means so as to be beneficial to the subsequent conversion and utilization of each component, the utilization efficiency of three components of the biomass is improved, and the biorefinery process of the lignocellulose biomass is realized.
In recent years, organic solvent pretreatment has been one of the main methods for achieving separation of components of lignocellulosic biomass. Patent CN106674538a discloses a method for separating and extracting cellulose, hemicellulose degrading sugar and lignin from bamboo, and provides a lignocellulose component separation process with gamma-valerolactone aqueous solution as solvent under the action of acid; patent ZL201510813243.1 discloses a green process for separating lignocellulose components, which is used for pretreating biomass by irradiation and coupling tetrahydrofuran or gamma-valerolactone reaction to realize the separation of lignocellulose components; patent ZL201410006095.8 discloses a method for preparing cellulose and lignin under normal pressure ultrasonic assistance by taking high-boiling alcohol as a solvent, and the cellulose and lignin in biomass are separated by digestion in a high-boiling alcohol solution at 130-140 ℃; patent ZL202010101379.0 discloses a method for efficiently separating lignocellulose by an ionic liquid-high-boiling alcohol composite system and carrying out enzymolysis, and the component separation efficiency of biomass is further improved by a multi-step composite pretreatment mode. Although the lignocellulose structure can be effectively broken through by the method for separating the components of the organic solvent to realize the partial or complete separation of the components, the high-efficiency component separation technology often needs higher reaction temperature (> 150 ℃), the multistep pretreatment method brings the complex process steps of solvent circulation, hemicellulose and lignin separation and the like, and the problems of high energy consumption and high environmental pressure are easily generated in the practical application process.
The invention comprises the following steps:
The invention solves the problems existing in the prior art, and provides a method for separating lignocellulose biomass components by pretreatment of an organic solution, which utilizes a triethylene glycol acid solution system to complete disassembly of hemicellulose and dissolution of lignin which are biomass raw materials in a mild environment, efficiently retains cellulose component filter residues, breaks a lignocellulose compact structure and realizes separation of all components in lignocellulose biomass.
The invention aims to provide a method for separating lignocellulose biomass components by pretreatment of an organic solvent, which comprises the following steps: adding lignocellulose biomass and triethylene glycol solution into a reaction vessel, wherein the triethylene glycol solution is a triethylene glycol aqueous solution containing an acid catalyst, reacting for 0.1-6 hours at 80-140 ℃, and then carrying out solid-liquid separation to obtain filter residues containing cellulose components and filtrate containing hemicellulose and lignin; adding an anti-solvent into the filtrate, carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover the anti-solvent and triethylene glycol solution; adding the filter residue containing lignin and hemicellulose components into hydrochloric acid solution, stirring, and performing solid-liquid separation to obtain lignin component residues and filtrate containing xylose and xylan.
Preferably, the mass volume ratio of the lignocellulose biomass to the triethylene glycol solution is 1: (8-20) g/mL.
Preferably, the volume fraction of 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 acid catalyst is soluble acid or strong acid weak alkali salt, wherein the acid is selected from one of sulfuric acid, hydrochloric acid, formic acid and methyl benzene sulfonic acid, and the strong acid weak alkali salt is selected from one of ferric sulfate, aluminum trichloride and copper nitrate.
Preferably, an anti-solvent is added to the filtrate in an amount of 8 times the volume of the filtrate, wherein the anti-solvent is diethyl ether.
Preferably, the mass volume ratio of the filter residue containing lignin and hemicellulose components to the hydrochloric acid solution is 1: the mass concentration of the hydrochloric acid solution is 1% in 10 g/mL.
Preferably, the particle size of the lignocellulose biomass is 0.5-3 mm.
Preferably, the lignocellulose biomass is an energy plant or waste containing at least cellulose and lignin. The energy plant comprises pennisetum and the like.
Further preferably, the waste is forestry waste, agricultural waste or processing waste. Forestry waste including wood dust and the like, agricultural waste including straw and the like, and processing waste including bagasse, furfural residue and the like are sugar refinery or winery processing waste.
Compared with the prior art, the invention has the following advantages:
(1) The invention utilizes the excellent lignin dissolving capability of acidic triethylene glycol to separate lignocellulose biomass under mild conditions, realizes the separation and recovery of raw material cellulose components and lignin components in the form of filter residues, and realizes the separation and recovery of hemicellulose components in the form of xylose and xylan.
(2) The filter residue rich in cellulose component obtained by the invention has high cellulose component content and is easy to be subjected to enzymolysis, conversion and utilization.
(3) The high-boiling triethylene glycol has good biocompatibility and low pressure in the reaction process.
(4) The invention has wide application range of raw materials, and the used solvent can be recycled, so that the cost can be effectively reduced.
The specific embodiment is as follows:
the following examples are further illustrative of the invention and are not intended to be limiting thereof.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention. Unless otherwise indicated, the experimental materials and reagents herein are all commercially available products conventional in the art.
Example 1
2G bagasse with granularity of 0.5mm (containing 40.1 percent of cellulose, 24.3 percent of hemicellulose and 18.2 percent of lignin) is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the sulfuric acid concentration of 0.2mol/L and the triethylene glycol volume fraction of 100% into a reactor in the amount of 8 g/mL; after reacting for 0.5h at 100 ℃, carrying out solid-liquid separation to obtain 1.02g of filter residue with the cellulose content of 71.8% (substrate concentration of 5%, CTec enzyme of 20FPU/g cellulose, enzymolysis for 72h at 50 ℃ and enzymolysis rate of 80.1%); adding diethyl ether with the volume of 8 times of the filtrate into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover diethyl ether and triethylene glycol solution; adding filter residues 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 residues to the dilute hydrochloric acid solution is 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.22g of lignin filter residues, and recovering 43.3% hemicellulose components in the form of soluble xylose and xylan.
Comparative example 1
Comparative example 1 was carried out 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 carried out as in example 1, except that polyethylene glycol 400 was used instead of triethylene glycol used in example 1.
Comparative example 3
Comparative example 3 was carried out as in example 1, except that the triethylene glycol used in example 1 was replaced with ethanol.
Comparative example 4
Comparative example 4 was carried out as in example 1, except that glycerol was used instead of triethylene glycol used in example 1.
The amounts of the filter residues and lignin recovered in example 1 and comparative examples 1 to 4 are shown in Table 1:
TABLE 1
| Filtering residues | Cellulose content of filter residue | Cellulose hydrolysis 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, the filter residue of the triethylene glycol solution has the highest cellulose content and the highest cellulose hydrolysis rate, which shows that the triethylene glycol solution has obvious advantages in separation performance of lignocellulose biomass components compared with the comparative alcohol solution.
Example 2
2G bagasse with granularity of 0.5mm (containing 40.1 percent of cellulose, 24.3 percent of hemicellulose and 18.2 percent of lignin) is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the sulfuric acid concentration of 0.05mol/L and the triethylene glycol volume fraction of 50% into a reactor in the amount of 8 g/mL; after reaction for 6 hours at 80 ℃, carrying out solid-liquid separation to obtain 1.36g of filter residue with 54.5% of cellulose (substrate concentration 5%, CTec enzyme of 20FPU/g cellulose, enzymolysis for 72 hours at 50 ℃ and enzymolysis rate of 43.3%); adding diethyl ether with the volume of 8 times of the filtrate into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover diethyl ether and triethylene glycol solution; adding filter residues 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 residues to the dilute hydrochloric acid solution is 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.16g of lignin filter residues, and recovering 30.8% of hemicellulose components in the form of soluble xylose and xylan.
Example 3
2G bagasse with granularity of 3.0mm (containing 40.1 percent of cellulose, 24.3 percent of hemicellulose and 18.2 percent of lignin) is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the sulfuric acid concentration of 0.2mol/L and the 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 (substrate concentration 5%, CTec enzyme of 20FPU/g cellulose, enzymolysis for 72h at 50 ℃ and enzymolysis rate 88.4%) of filter residue with 86.9% cellulose; adding diethyl ether with the volume of 8 times into the filtrate, carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover diethyl ether and triethylene glycol solution; adding filter residues 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 residues to the dilute hydrochloric acid solution is 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.23g of lignin filter residues, and recovering 46.7% of hemicellulose components in the form of soluble xylose and xylan.
Example 4
2G bagasse with granularity of 3.0mm (containing 40.1 percent of cellulose, 24.3 percent of hemicellulose and 18.2 percent of lignin) is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the sulfuric acid concentration of 0.1mol/L and the triethylene glycol volume fraction of 100% into a reactor in an amount of 20 g/mL; after reacting for 2 hours at 100 ℃, carrying out solid-liquid separation to obtain 0.83g of filter residue with the cellulose content of 90.5% (substrate concentration of 5%, CTec enzyme of 20FPU/g cellulose, and carrying out enzymolysis for 72 hours at 50 ℃ with the enzymolysis rate of 91.7%); adding diethyl ether with the volume of 8 times of the filtrate into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover an anti-solvent and a triethylene glycol solution; adding filter residues 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 residues to the dilute hydrochloric acid solution is 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.26g of lignin filter residues, and recovering 52.3% hemicellulose components in the form of soluble xylose and xylan.
Example 5
2G of furfural residue (containing 36.4 percent of cellulose, 1.2 percent of hemicellulose and 34.5 percent of lignin) with granularity of 0.5mm is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the hydrochloric acid concentration of 0.1mol/L and the triethylene glycol volume fraction of 100% into a reactor in the amount of 10 g/mL; after reacting for 2 hours at 100 ℃, carrying out solid-liquid separation to obtain 0.86g (substrate concentration 5%, CTec enzyme of 20FPU/g cellulose, enzymolysis for 72 hours at 50 ℃ and enzymolysis rate of 84.5%) of filter residue with the cellulose content of 79.9%; adding diethyl ether with the volume of 8 times of the filtrate into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover an anti-solvent and a triethylene glycol solution; adding the 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 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.23g of lignin filter residue.
Example 6
2G of poplar (containing 46.1% of cellulose, 12.7% of hemicellulose and 24.4% of lignin) with granularity of 0.5mm is taken as a raw material, and the mass volume ratio of the raw material to the triethylene glycol solution is 1: adding triethylene glycol solution with the concentration of aluminum chloride of 0.1mol/L and the volume fraction of triethylene glycol of 100% into a reactor in an amount of 10 g/mL; after reacting for 2 hours at 100 ℃, carrying out solid-liquid separation to obtain 1.32g of filter residue with the cellulose content of 64.8% (substrate concentration of 5%, CTec enzyme of 20FPU/g cellulose, and carrying out enzymolysis for 72 hours at 50 ℃ with the enzymolysis rate of 55.3%); adding diethyl ether with the volume of 8 times of the filtrate into the filtrate, and carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover diethyl ether and triethylene glycol solution; adding filter residues 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 residues to the dilute hydrochloric acid solution is 1:10g/mL, stirring at 60 ℃ for 2 hours, and then carrying out solid-liquid separation to obtain 0.15g of lignin filter residues, and recovering 31.6% hemicellulose components in the form of soluble xylose and xylan.
The above embodiments are only described to assist in understanding the technical solution of the present invention and its core idea, and it should be noted that it will be obvious to those skilled in the art that several improvements and modifications can be made 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 (5)
1. A method for separating components of lignocellulose biomass by pretreatment of an organic solvent, which is characterized by comprising the following steps: adding lignocellulose biomass and triethylene glycol solution into a reaction vessel, wherein the triethylene glycol solution is the triethylene glycol solution containing an acid catalyst, reacting for 0.1-6 hours at 80-140 ℃, and then carrying out solid-liquid separation to obtain filter residues containing cellulose components and filtrate containing hemicellulose and lignin; adding an anti-solvent with the volume of 8 times of that of the filtrate into the filtrate, wherein the anti-solvent is diethyl ether, carrying out solid-liquid separation to obtain filter residues containing lignin and hemicellulose components, and carrying out reduced pressure distillation on the filtrate to recover the anti-solvent and triethylene glycol solution; adding filter residues containing lignin and hemicellulose components into hydrochloric acid solution, stirring, and performing solid-liquid separation to obtain lignin component residues and filtrate containing xylose and xylan; the mass volume ratio of the lignocellulose biomass to the triethylene glycol solution is 1: (8-20) g/mL; the volume fraction of triethylene glycol in the triethylene glycol solution is 50% -100%, and the concentration of the acid catalyst is 0.05-0.20 mol/L; the acid catalyst is soluble acid or strong acid weak alkali salt, wherein the acid is selected from one of sulfuric acid, hydrochloric acid, formic acid and methyl benzene sulfonic acid, and the strong acid weak alkali salt is selected from one of ferric sulfate, aluminum trichloride and copper nitrate.
2. The method according to claim 1, wherein the mass to volume ratio of the filter residue containing lignin and hemicellulose components to the hydrochloric acid solution is 1: the mass concentration of the hydrochloric acid solution is 1% in 10 g/mL.
3. The method of claim 1, wherein the lignocellulosic biomass has a particle size of 0.5 to 3mm.
4. The method of claim 1, wherein the lignocellulosic biomass is an energy plant or waste comprising at least cellulose and lignin.
5. The method of claim 4, wherein the waste is forestry waste, agricultural waste or processing waste.
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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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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