CN112342044A - Method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass - Google Patents
Method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
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Abstract
The invention discloses a method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass. The method comprises the following steps: (1) uniformly mixing the biomass with a liquid acid catalyst or a solid acid catalyst to obtain a mixture; (2) carrying out low-temperature pyrolysis on the mixture to obtain low-temperature pyrolysis solid residue and steam, and condensing and collecting the steam; (3) and (3) mixing and drying the low-temperature pyrolysis solid residue and an activating agent, performing medium-high temperature pyrolysis to obtain biochar, steam and uncondensable pyrolysis gas, condensing and collecting the steam, and combusting the uncondensable pyrolysis gas for drying the biomass in the step (1) and pyrolyzing the biomass in the step (2) at a low temperature. The method provided by the invention realizes the directional conversion of cellulose and hemicellulose in biomass to prepare dehydrated sugar and derivatives thereof in a low-temperature pyrolysis stage, and the lignin-rich solid residue obtained in the low-temperature pyrolysis stage is mixed with an activating agent and then subjected to medium-high temperature fast pyrolysis to directionally prepare biochar.
Description
Technical Field
The invention relates to the technical field of chemical engineering and energy engineering, in particular to a method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass.
Background
Fast pyrolysis of biomass is a simple, low-cost, and efficient thermochemical conversion technique to rapidly convert solid biomass into high-yield liquid bio-oil. Fast pyrolysis of biomass is to maximize the yield of bio-oil, which can be as high as 60-75 wt.%, by means of medium temperature (400-600 ℃), high heating rate (>1000 ℃/s) and short gas phase residence time (<2 s). Although the yield of the bio-oil is high, the composition of the bio-oil is very complex, mainly comprises water and hundreds of oxygen-containing organic compounds, and the concentration of most of the oxygen-containing organic compounds is lower than 2 wt.%, so that the quality of the bio-oil is low, and the further purification of chemicals or catalytic upgrading is difficult. The complex composition of bio-oil is mainly due to the heterogeneous structure of biomass and the high temperatures present during fast pyrolysis in combination with the catalytic action of alkali/alkaline earth metals (Na, K, Ca and Mg). The biomass mainly comprises three components of cellulose, hemicellulose and lignin, and a small amount of extracts and inorganic ash, and the difference of the thermal stability and the distribution of pyrolysis products is obvious due to the structural difference of the three components of the biomass. The high temperatures present during pyrolysis and the catalytic action of alkali/alkaline earth metals in the ash promote C-C bond cleavage (e.g., ring opening and decarbonylation/decarboxylation reactions) in the biomass, further exacerbating the complexity of the bio-oil component. There is therefore an urgent need to develop new pyrolysis processes to achieve directional conversion of biomass.
Disclosure of Invention
The invention provides a method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass.
The invention aims to provide a method for directionally preparing chemicals and biochar by controllable graded catalytic pyrolysis of biomass, which comprises the following steps:
(1) uniformly mixing the biomass with a liquid acid catalyst or a solid acid catalyst to obtain a mixture;
(2) carrying out low-temperature pyrolysis on the mixture obtained in the step (1) in a low-temperature pyrolysis reactor to obtain low-temperature pyrolysis solid residues and steam, and condensing and collecting the steam;
(3) and (3) mixing and drying the low-temperature pyrolysis solid residue obtained in the step (2) with an activating agent, introducing into a fast pyrolysis reactor for medium-high temperature pyrolysis to obtain biochar, steam and non-condensable pyrolysis gas, condensing and collecting the steam, and combusting the non-condensable pyrolysis gas for drying the biomass in the step (1) and pyrolyzing the biomass in the step (2) at a low temperature.
The method for realizing the oriented preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass firstly carries out low-temperature pyrolysis, and mixes the low-temperature pyrolysis solid residue with an activating agent and then carries out medium-high temperature fast pyrolysis to realize the oriented preparation of chemicals and biochar by the graded quality of biomass, thereby realizing the resource utilization of biomass.
The biomass is harvested and crushed to the particle size of less than 1cm, and the crushed biomass is uniformly mixed with a liquid acid catalyst or a solid acid catalyst to obtain a mixture. The solid-liquid mixture obtained by the biomass and the liquid acid catalyst is directly dried at 40 ℃ to 80 ℃ (preferably 60 ℃). Solid acid catalysts or liquid acid catalysts are mainly used for passivating minerals in biomass: such as alkali and alkaline earth metals, while achieving low temperature activation and directional conversion of cellulose and hemicellulose.
Preferably, the collected liquid products condensed in step (2) and step (3) are the chemicals produced. Low-temperature pyrolysis directionally converts cellulose and hemicellulose in the biomass into dehydrated sugar and derivatives thereof; and (3) converting lignin and a small amount of residual unconverted cellulose and hemicellulose in the low-temperature pyrolysis solid residue into phenolic compounds and biochar by medium-high temperature pyrolysis. The low-temperature pyrolysis liquid product is rich in dehydrated sugar and derivatives thereof, and the fast pyrolysis liquid product is rich in phenolic compounds. The solid product produced in the fast pyrolysis reactor is biochar.
Preferably, the liquid acid catalyst in the step (1) is selected from one of a sulfuric acid solution, a hydrochloric acid solution, a sulfonic acid solution, a phosphoric acid solution, a nitric acid solution, a formic acid solution and an acetic acid solution, the load capacity of the liquid acid catalyst accounts for 0.01-15% of the mass of the biomass, and the solid-to-liquid ratio of the biomass to the liquid acid catalyst is 5-10: 1; the carrier of the solid acid catalyst is selected from one of silicon dioxide, aluminum oxide, ferroferric oxide, biochar, titanium dioxide, zirconium dioxide and a molecular sieve, the acid is selected from one of sulfuric acid, hydrochloric acid, sulfonic acid and phosphoric acid, the load capacity of the acid accounts for 0.01-50% of the mass of the carrier, and the mass ratio of the solid catalyst to the biomass is 0.1-10.
Preferably, the biomass in the step (1) is agricultural biomass, forestry biomass, industrial biomass waste or cellulose or hemicellulose obtained by pretreating the waste.
Preferably, the low-temperature pyrolysis temperature in the step (2) is 200-350 ℃, and the low-temperature pyrolysis atmosphere is nitrogen, argon, carbon dioxide, water vapor or flue gas. Further preferably, the low-temperature pyrolysis temperature is 280 ℃ to 320 ℃.
Preferably, the solid-phase residence time of the mixture in the step (2) in the low-temperature pyrolysis reactor is 1-3600 s.
Preferably, the medium-high temperature pyrolysis temperature in the step (3) is 400-800 ℃, and the medium-high temperature pyrolysis atmosphere is nitrogen, argon, water vapor, carbon dioxide or flue gas; the activating agent is phosphoric acid solution, zinc chloride solution or potassium hydroxide solution, and the mass ratio of the activating agent to the low-temperature pyrolysis solid residue is (0-1000): 1. the mass fraction of the phosphoric acid solution, the zinc chloride solution or the potassium hydroxide solution is 5 to 99 percent.
Further preferably, the mass ratio of the activating agent to the low-temperature pyrolysis solid residue is 100-500: 1, the medium-high temperature pyrolysis temperature is 500-600 ℃.
Preferably, the solid phase residence time of the low-temperature pyrolysis solid residue in the fast pyrolysis reactor in the step (3) is 0.1 to 300 s. Further preferably, the solid-phase retention time of the low-temperature pyrolysis solid residue in the fast pyrolysis reactor is 1-20 s.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts the solid acid catalyst or the liquid acid catalyst to be uniformly mixed with the biomass to realize the low-temperature activation and the directional conversion of cellulose and hemicellulose in the biomass, thereby preparing the high-yield, high-selectivity and high-added-value chemicals.
2. The invention prepares phenolic chemicals and biochar by medium-high temperature fast pyrolysis and orientation after mixing lignin-rich solid residue and an activating agent.
Drawings
FIG. 1 is a process flow diagram of the method for realizing the directional preparation of chemicals and biochar by biomass controllable graded catalytic pyrolysis.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof. The equipment and reagents used in the present invention are, unless otherwise specified, conventional commercial products in the art.
Example 1
Crushing the corn cob to 60-80 meshes, putting the crushed corn cob into a sulfuric acid solution, stirring and dipping for 12 hours at normal temperature, and then carrying out ultrasonic treatment for 2 hours. The dipping amount of the sulfuric acid is 2.75 percent of the mass of the corncobs, and the solid-to-liquid ratio during dipping is 1: 10. the corn cob dipped with the sulfuric acid is directly put into an oven to be dried at 60 ℃. And (2) carrying out normal-pressure low-temperature pyrolysis on the dried corn cobs loaded with sulfuric acid in a spiral reactor, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 300 ℃, the solid-phase retention time is 5min, so as to obtain solid residues and low-temperature pyrolysis steam, the low-temperature pyrolysis steam is condensed at-40 ℃ through a condensing tube so as to obtain dehydrated sugar and derivatives thereof, and the dehydrated sugar and the derivatives thereof are detected to be levoglucosan, 1, 5-dehydration-beta-xylofuranose, furfural and levoglucosenone respectively.
Compared with untreated corncobs, the mass yields of L-glucan, 1, 5-anhydro-beta-xylofuranose, furfural and L-glucosone produced by the corncobs after the treatment of the loaded sulfuric acid can be rapidly increased from 1.3%, 0.1%, 0.3% and 0.1% to 18.9%, 4.6%, 4.8% and 1.7% respectively.
Mixing and drying the solid residue obtained by low-temperature pyrolysis and a phosphoric acid solution, placing the mixture in a bubbling fluidized bed for normal-pressure fast pyrolysis, wherein the mass ratio of phosphoric acid to the solid residue is 2: 1, the mass fraction of phosphoric acid in the phosphoric acid solution is 30%, the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 550 ℃, the solid phase retention time is about 5s, and the fast pyrolysis steam is condensed at-40 ℃ through a condensing tube to obtain the phenolic chemicals and the biochar, wherein the yield of the biological oil rich in the phenolic chemicals is 14%, and the yield of the biochar is 45%. The fast pyrolysis non-condensable pyrolysis gas is combusted for low-temperature pyrolysis and drying heat supply.
Example 2
Crushing eucalyptus wood into 80-100 meshes, putting the crushed eucalyptus wood into a formic acid solution, stirring and soaking for 12 hours at normal temperature, and then carrying out ultrasonic treatment for 2 hours. The impregnation amount of formic acid is 0.7 percent of the mass of the eucalyptus, and the solid-liquid ratio during impregnation is 1: 5. the eucalyptus wood soaked with the hydrochloric acid is directly put into an oven to be dried at 60 ℃. And (2) carrying out normal-pressure low-temperature pyrolysis on the dried eucalyptus wood loaded with formic acid in a fixed bed reactor, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 300 ℃, the solid-phase retention time is 4min, so as to obtain solid residues and low-temperature pyrolysis steam, the low-temperature pyrolysis steam is condensed at-40 ℃ through a condenser pipe so as to obtain dehydrated sugar and derivatives thereof, and the dehydrated sugar and the derivatives thereof are detected to be levoglucosan, 1, 5-dehydration-beta-xylofuranose, furfural and levoglucosenone respectively.
Compared with untreated eucalyptus wood, the mass yields of the levoglucosan, 1, 5-anhydro-beta-xylofuranose, furfural and levoglucosenone generated by the eucalyptus wood after the treatment of the impregnated formic acid are rapidly increased from 4.1%, 0.1%, 0.6%, 0.1% to 20.2%, 5.5%, 6.8% and 1.7%, respectively.
Mixing and drying the solid residue obtained by low-temperature pyrolysis and a zinc chloride solution, and then carrying out normal-pressure rapid pyrolysis in a bubbling fluidized bed, wherein the mass ratio of zinc chloride to the solid residue is 2: 1, the pyrolysis atmosphere is nitrogen, the mass fraction of zinc chloride in a zinc chloride solution is 30%, the pyrolysis temperature is 600 ℃, the solid phase retention time is about 5s, and the fast pyrolysis steam is condensed at the temperature of minus 40 ℃ through a condensing tube to obtain phenolic chemicals and biochar, wherein the yield of the biological oil rich in the phenolic chemicals is 8%, and the yield of the biochar is 42%. The fast pyrolysis non-condensable pyrolysis gas is combusted for low-temperature pyrolysis and drying heat supply.
Example 3
Crushing pine wood to 80-100 meshes, putting the crushed eucalyptus wood into a phosphoric acid solution, stirring and soaking for 12 hours at normal temperature, and then carrying out ultrasonic treatment for 2 hours. The impregnation amount of the phosphoric acid is 0.30 percent of the mass of the eucalyptus wood, and the solid-liquid ratio during impregnation is 1: 5. the eucalyptus wood soaked with the phosphoric acid is directly put into an oven to be dried at 60 ℃. And (2) pyrolyzing the dried eucalyptus wood loaded with phosphoric acid at normal pressure and low temperature in a fixed bed reactor, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 300 ℃, the solid phase retention time is 4min, so as to obtain solid residues and low-temperature pyrolysis steam, the low-temperature pyrolysis steam is condensed at-40 ℃ through a condenser pipe so as to obtain dehydrated sugar and derivatives thereof, and the dehydrated sugar and the derivatives thereof are detected to be levoglucosan, 1, 5-dehydration-beta-xylofuranose, furfural and levoglucosenone respectively.
Compared with untreated pine, the quality yield of the L-glucan, 1, 5-dehydration-beta-xylofuranose, furfural and L-glucosone generated by the eucalyptus wood is rapidly increased from 5.2%, 0.1%, 0.4% and 0% to 30.2%, 3.5%, 0.9% and 1.2% respectively after the phosphoric acid impregnation treatment.
Mixing and drying solid residues obtained by low-temperature pyrolysis and a phosphoric acid solution, and then performing normal-pressure fast pyrolysis in a bubbling fluidized bed, wherein the mass ratio of phosphoric acid to the solid residues is 2: 1, the pyrolysis atmosphere is nitrogen, the mass fraction of phosphoric acid in the phosphoric acid solution is 30%, the pyrolysis temperature is 600 ℃, the solid phase retention time is about 5s, and the fast pyrolysis steam is condensed at-40 ℃ through a condensing tube to obtain the phenolic chemicals and the biochar, wherein the yield of the biological oil rich in the phenolic chemicals is 5%, and the yield of the biological coke is 46%. The fast pyrolysis non-condensable pyrolysis gas is combusted for low temperature pyrolysis and dry heat supply.
Example 4
And (2) putting the zirconia carrier into a sulfuric acid solution for saturated impregnation, wherein the loading amount of sulfuric acid is 2 wt.%, drying to obtain a sulfuric acid catalyst loaded on zirconia, and drying at 105 ℃ for 12 hours for later use. Crushing pine wood to 80-100 meshes, and mixing the crushed pine wood and a catalyst according to the weight ratio of 1: 1, and uniformly mixing. And (2) pyrolyzing the mixture of the pine and the catalyst at normal pressure and low temperature in a fixed bed reactor, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 300 ℃, the solid phase retention time is 6min, so as to obtain solid residues and low-temperature pyrolysis steam, and the low-temperature pyrolysis steam is condensed at-40 ℃ through a condensing tube so as to obtain chemicals such as levoglucosan, 1, 5-dehydration-beta-xylofuranose, furfural, levoglucosenone and the like. And (3) carrying out normal-pressure fast pyrolysis on the solid residue obtained by low-temperature pyrolysis in a bubbling fluidized bed, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 550 ℃, the solid-phase retention time is about 5s, and fast pyrolysis steam is condensed at-40 ℃ through a condensing tube to obtain the phenol chemicals and the biochar, wherein the yield of the bio-oil rich in the phenol chemicals is 21%, and the yield of the biochar is 28%. The fast pyrolysis non-condensable pyrolysis gas is used for low-temperature pyrolysis and drying heat supply respectively after being combusted.
Example 5
The corn straws are crushed into 60-80 meshes, and the crushed corn straws are put into 2mol/l hydrochloric acid solution and stirred for 24 hours at normal temperature to remove ash. The ash-removed corn straws are put into a sulfuric acid solution again to be stirred and dipped for 12 hours at normal temperature, and then are subjected to ultrasonic treatment for 2 hours. The dipping amount of the sulfuric acid is 0.1 percent of the mass of the corn straws, and the solid-to-liquid ratio during dipping is 1: 10. the maize straws soaked with the sulfuric acid are directly put into an oven to be dried at 60 ℃. And (2) carrying out normal-pressure low-temperature pyrolysis on the dried corn straw loaded with sulfuric acid in a spiral reactor, wherein the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 300 ℃, the solid phase retention time is 5min, so as to obtain solid residues and low-temperature pyrolysis steam, and the low-temperature pyrolysis steam is condensed at-40 ℃ through a condensing tube so as to obtain dehydrated sugar and derivatives thereof, wherein the mass yields of levoglucosan, 1, 5-dehydration-beta-xylofuranose, furfural and levoglucosenone are respectively 15.1%, 4.9%, 4.3% and 1.6%. Mixing and drying solid residues obtained by low-temperature pyrolysis and a potassium hydroxide solution, and then performing normal-pressure fast pyrolysis in a bubbling fluidized bed, wherein the mass ratio of potassium hydroxide to the solid residues is 2: 1, the pyrolysis atmosphere is nitrogen, the pyrolysis temperature is 550 ℃, the solid phase retention time is about 5s, and the fast pyrolysis steam is condensed at-40 ℃ through a condensing tube to obtain the phenol chemicals and the biochar, wherein the yield of the biological oil rich in the phenol chemicals is 6%, and the yield of the biological coke is 42%. The fast pyrolysis non-condensable pyrolysis gas is combusted for low temperature pyrolysis and dry heat supply.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (9)
1. A method for realizing the directional preparation of chemicals and biochar by biomass controllable graded catalytic pyrolysis is characterized by comprising the following steps:
(1) uniformly mixing the biomass with a liquid acid catalyst or a solid acid catalyst to obtain a mixture;
(2) performing low-temperature pyrolysis on the mixture obtained in the step (1) to obtain low-temperature pyrolysis solid residue and steam, and condensing and collecting the steam;
(3) and (3) mixing and drying the low-temperature pyrolysis solid residue obtained in the step (2) with an activating agent, performing medium-high temperature pyrolysis to obtain biochar, steam and non-condensable pyrolysis gas, condensing and collecting the steam, and combusting the non-condensable pyrolysis gas for drying the biomass in the step (1) and performing low-temperature pyrolysis on the biomass in the step (2).
2. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, characterized in that the collected liquid products in the steps (2) and (3) are condensed into the prepared chemicals.
3. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the liquid acid catalyst in the step (1) is selected from one of sulfuric acid solution, hydrochloric acid solution, sulfonic acid solution, phosphoric acid solution, nitric acid solution, formic acid solution and acetic acid solution, the load of the liquid acid catalyst accounts for 0.01-15% of the mass of the biomass, and the solid-to-liquid ratio of the biomass to the liquid acid catalyst is 5-10: 1; the carrier of the solid acid catalyst is selected from one of silicon dioxide, aluminum oxide, ferroferric oxide, biochar, titanium dioxide, zirconium dioxide and a molecular sieve, the acid is selected from one of sulfuric acid, hydrochloric acid, sulfonic acid and phosphoric acid, the load capacity of the acid accounts for 0.01-50% of the mass of the carrier, and the mass ratio of the solid catalyst to the biomass is 0.1-10.
4. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the biomass in the step (1) is agricultural biomass, forestry biomass, industrial biomass waste or cellulose or hemicellulose obtained by the pretreatment of the waste.
5. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the low-temperature pyrolysis temperature in the step (2) is 200-350 ℃, and the low-temperature pyrolysis atmosphere is nitrogen, argon, carbon dioxide, water vapor or flue gas.
6. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the solid-phase residence time of the mixture in the step (2) in a low-temperature pyrolysis reactor is 1-3600 s.
7. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, characterized in that the medium-high temperature pyrolysis temperature in the step (3) is 400-800 ℃, and the medium-high temperature pyrolysis atmosphere is nitrogen, argon, water vapor, carbon dioxide or flue gas.
8. The method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the activating agent in the step (3) is phosphoric acid solution, zinc chloride solution or potassium hydroxide solution, and the mass ratio of the activating agent to the low-temperature pyrolysis solid residue is 0-1000: 1.
9. the method for realizing the directional preparation of chemicals and biochar by the controllable graded catalytic pyrolysis of biomass according to claim 1, wherein the solid-phase retention time of the low-temperature pyrolysis solid residue in the fast pyrolysis reactor in the step (3) is 0.1-300 s.
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| CN114950364A (en) * | 2022-05-23 | 2022-08-30 | 四川大学 | Biomass fast pyrolysis residue-based porous carbon sphere and preparation method and application thereof |
| CN115806284A (en) * | 2022-10-21 | 2023-03-17 | 中科(宜兴)新材料研究有限公司 | Preparation method for improving yield of biomass-based hard carbon |
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