Method for separating and extracting Juncao biomass components
By combining hydrothermal methods with mixed catalysts, the problem of separating cellulose, hemicellulose, and lignin in Juncao (a type of grass) has been solved, achieving efficient separation and high-value utilization, and enhancing the utilization value of Juncao resources.
Patent Information
- Application Number
- CN202511228817.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-29
- Publication Date
- 2025-12-12
AI Technical Summary
Existing technologies are insufficient for efficiently separating and utilizing the three major components of Juncao (a type of grass), namely cellulose, hemicellulose, and lignin, resulting in resource waste and insufficient utilization value.
A method combining hydrothermal treatment and mixed catalysts was adopted to achieve efficient separation of Juncao biomass components through hydrolysis and mixed catalyst treatment. The process includes steps such as hydrolysis, centrifugation, drying and alcohol washing. The catalyst was prepared by mixing choline chloride, acid and catalyst in a ratio of 1:1:0.2.
It achieves efficient separation of the three components, improves the removal rate and purity, simplifies the operation, reduces costs, and preserves the active structure of cellulose, making it suitable for subsequent high-value utilization.
Smart Images
Figure CN121108518A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of plant component separation and extraction technology, specifically relating to a method for separating and extracting components from Juncao biomass. Background Technology
[0002] In the context of contemporary socio-economic development and energy shortages, biomass has significant research importance and great utilization value.
[0003] After years of innovation, Juncao has been widely used in the forefront of sustainable development, such as desertification control, animal husbandry, board making, papermaking, and power generation.
[0004] Juncao (a type of grass) is mainly composed of three components: hydrophobic lignin, hydrophilic hemicellulose, and structurally amphiphilic cellulose. Cellulose molecules intertwine into bundles, dispersed within the hemicellulose and lignin components, forming a structure similar to reinforced concrete. This structure plays a supporting and protective role in Juncao's growth, but it also makes it difficult to separate the three components physically. While chemical treatments using acids, alkalis, and organic solvents can achieve partial separation of lignin, hemicellulose, and cellulose, usually only one or two components (primarily cellulose) can be utilized, making it difficult to achieve high-value utilization of all three components. Furthermore, this single utilization mode inevitably leads to significant waste of the other components.
[0005] Therefore, there is an urgent need to develop a new method to achieve efficient separation and transformation of the three major components and expand the application value of Juncao. Summary of the Invention
[0006] The purpose of this invention is to provide a method for separating and extracting components from Juncao biomass. The method provided by this invention can effectively separate cellulose, hemicellulose and lignin, and realize the high-value utilization of these three elements.
[0007] To achieve the above objectives, the present invention provides the following technical solution:
[0008] This invention provides a method for separating and extracting components from Juncao biomass. The method includes using Juncao as raw material and combining it with a hydrothermal method and a mixed catalyst to separate and extract Juncao cellulose, hemicellulose and lignin.
[0009] The mixed catalyst is prepared by mixing choline chloride, acid and catalyst in a ratio of 1:1:0.2 and heating and stirring at 100°C.
[0010] Preferably, the acid is lactic acid, oxalic acid, citric acid, malic acid, formic acid, or acetic acid; and the catalyst is ZnCl2 or FeCl3.
[0011] The present invention also provides a method for separating and extracting components from Juncao biomass, which specifically includes the following steps:
[0012] S1. Mix the Juncao granules with desalinated water and carry out a hydrolysis reaction. After the hydrolysis reaction is completed, the products are separated by filtration to obtain hydrolysate and hydrolysis residue respectively.
[0013] S2. The hydrolysate is centrifuged multiple times, the supernatant is collected, and dried at low temperature to obtain the water-soluble hemicellulose component.
[0014] S3. After drying, the hydrolysis residue is mixed with the mixed catalyst solution. After the reaction is completed, the residue is filtered and washed to obtain cellulose. The filtrate is then washed with alcohol, water and dried to obtain lignin.
[0015] The mixed catalyst is prepared by mixing choline chloride, acid and catalyst in a ratio of 1:1:0.2 and heating and stirring at 100°C.
[0016] Preferably, the mixing ratio of the fungal grass granules and the desalinated water in step S1 is 1:(5-12); the conductivity of the desalinated water is 0.7 μs / cm, pH 7.2, sodium ion concentration is 30 μg / L, and the silicate concentration of the desalinated water is 40 μg / L.
[0017] Preferably, the hydrolysis reaction in step S1 includes a low-temperature pretreatment process at 120-140℃ and a high-temperature reaction process at 160-180℃ for 0.5-2 hours after adding an inhibitor, with a total pressure of 1 MPa throughout the reaction.
[0018] Preferably, the inhibitor is EDTA or glutamic acid-N,N-diacetic acid; the amount of the inhibitor added is 0.01-0.05 times the mass of the Juncao powder.
[0019] Preferably, the low-temperature drying condition in step S2 is 40°C.
[0020] Preferably, the reaction in step S3 is carried out in a water bath at 70-120°C with stirring for 1-5 hours.
[0021] Preferably, the alcohol washing process in step S3 involves mixing the filtrate with 95% ethanol at a volume ratio of 1:3, letting it stand for 2 hours, then centrifuging it, washing it with water, and freeze-drying it. The resulting solid product is the lignin component.
[0022] The beneficial effects of this invention are:
[0023] This invention utilizes a hydrothermal method to selectively dissolve hemicellulose in lignocellulose, using only water as a medium without adding any chemicals. It is simple to operate, low in cost, and clean and pollution-free.
[0024] This invention overcomes the shortcomings of traditional and existing processes by using a hydrothermal method in conjunction with a mixed catalyst solution, and greatly improves the removal rate of the three elements.
[0025] This invention achieves efficient separation of cellulose components from grass while retaining its own active aryl ether structure, which is beneficial for subsequent catalytic depolymerization of lignin. Attached Figure Description
[0026] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0027] Figure 1 This is a flowchart of the separation process for the components of Juncao biomass. Detailed Implementation
[0028] This invention provides a method for separating and extracting components from Juncao biomass.
[0029] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid particles using a pulverizer for storage and later use. The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:(5-12). (The desalinated water had a conductivity of 0.7 μs / cm, pH 7.2, sodium ion concentration of 30 μg / L, and silicate concentration of 40 μg / L). The pressure was set to 1 MPa. The mixture was first pretreated at low temperature (120-140℃) for 30 min to remove easily degradable components such as pectin. Then, an inhibitor (EDTA or glutamic acid-N,N-diacetic acid) was added. The ratio of Juncao powder to inhibitor was 1:(0.01-0.05). The mixture was reacted at high temperature (160℃-180℃) for 0.5-2 h to directionally extract hemicellulose and reduce excessive degradation. After the reaction was completed, the hydrolysis pot was removed. After the material cooled to room temperature, it was filtered and separated to obtain hydrolysate A1 and hydrolysis residue A2. Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature to form hemicellulose powder. The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0030] The prepared hydrolysis residue A2 was mixed with the prepared mixed catalyst solution at a solid-liquid ratio of 1:10 to 1:20 and placed in a flat-bottomed flask. The mixture was then placed in a water bath at 70℃ to 120℃ and stirred for 1-5 hours. After the reaction, the mixture was filtered and washed, and the filter residue was cellulose. The filtrate was then washed with alcohol and water several times and dried to obtain lignin.
[0031] The preparation process of the mixed catalyst solution is as follows: choline chloride, acid (which may include, but is not limited to, lactic acid, oxalic acid, citric acid, malic acid, formic acid or acetic acid), and catalyst (ZnCl2 or FeCl3) are mixed in a ratio of 1:1:0.02 and heated and stirred at 100°C until the solution is uniform and transparent.
[0032] Furthermore, the cellulose extracted by this invention can be dissolved and spun into regenerated cellulose filaments; the hemicellulose can be used as a raw material for the production of ethanol, glycopolymers and chemicals; and the lignin can be used as an oxidant in cosmetics or pharmaceutical preparations.
[0033] This invention first selectively dissolves hemicellulose from lignocellulose using a hydrothermal method, employing only water as the medium without adding any chemicals. The process is simple, low-cost, clean, and pollution-free. Simultaneously, it minimizes cellulose hydrolysis and sugar degradation reactions, and the absence of other solvents facilitates subsequent separation of cellulose and lignin, improving extract purity. The mixed catalyst exhibits good retention of cellulose components, swelling them to dissolve and separate lignin as much as possible, thus improving cellulose accessibility. The combined use of hydrothermal technology and mixed catalyst technology overcomes the shortcomings of traditional and existing processes, significantly improving the removal rate of hemicellulose, lignin, and lignin.
[0034] This invention reduces excessive degradation of hemicellulose, inhibits side reactions, avoids the formation of harmful inhibitors, and improves the purity of the hydrolysate by adding inhibitors. By adding catalysts (ZnCl2, FeCl3) to modify lignin in the fungus, specific chemical bonds in the lignin are directionally broken, improving its solubility and achieving efficient separation from cellulose components. Simultaneously, the active aryl ether structure is preserved, facilitating subsequent catalytic depolymerization for high-value lignin production.
[0035] To further illustrate the present invention, the technical solutions provided by the present invention will be described in detail below with reference to the accompanying drawings and embodiments, but these should not be construed as limiting the scope of protection of the present invention.
[0036] Unless otherwise specified, the production processes, experimental methods, or testing methods involved in the embodiments of this invention are all conventional methods in the prior art, and their names and / or abbreviations are all conventional names in the field, which are very clear and distinct in the relevant application areas. Those skilled in the art can understand the conventional process steps based on the names and apply the corresponding equipment, and implement them according to conventional conditions or the conditions recommended by the manufacturer.
[0037] The various instruments, equipment, raw materials or reagents used in the embodiments of this invention are not subject to any special restrictions on their source. They are all conventional products that can be purchased through regular commercial channels and can be prepared according to conventional methods known to those skilled in the art.
[0038] Example 1
[0039] The mature Juncao fiber raw material is processed by removing leaves, cutting into sections, washing, drying, and then pulverizing into solid granules for storage. The flow chart for separating Juncao biomass components is shown below. Figure 1 As shown.
[0040] The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The pressure was set to 1 MPa. The mixture was first pretreated at a low temperature of 120℃ for 30 minutes to remove easily degradable components such as pectin. Then, the inhibitor EDTA (the ratio of Juncao granules to inhibitor was 1:0.02) was added and reacted at a constant temperature of 165℃ for 1 hour. After the reaction was completed, the mixture was filtered to obtain hydrolysate A1 and hydrolysis residue A2.
[0041] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature (40℃) to form hemicellulose powder. The hemicellulose removal rate was 89.9% and the purity was 94.3%.
[0042] The hydrolysis residue A2 was washed multiple times with distilled water and dried at 105°C to constant weight (constant weight is defined as the difference in mass between two consecutive drying processes being less than 0.3 mg). It was then stored in an oven for later use.
[0043] Choline chloride, citric acid, and ZnCl2 were mixed in a molar ratio of 1:1:0.2 and heated and stirred at 100°C until a transparent solution was obtained. The hydrolysis residue A2 was mixed with the mixed catalyst solution in a solid-liquid ratio of 1:20 and stirred at 80°C for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 92.4% and 94.4%, respectively, with purities of 96.3% and 94.2%, respectively.
[0044] Example 2
[0045] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid particles using a pulverizer for storage and later use.
[0046] The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The pressure was set to 1 MPa. The mixture was first pretreated at a low temperature of 120℃ for 30 minutes to remove easily degradable components such as pectin. Then, the inhibitor EDTA (the ratio of Juncao granules to inhibitor was 1:0.02) was added and reacted at a constant temperature of 165℃ for 1 hour. After the reaction was completed, the mixture was filtered to obtain hydrolysate A1 and hydrolysis residue A2.
[0047] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature (40℃) to form hemicellulose powder. The hemicellulose removal rate was 89.9% and the purity was 94.3%.
[0048] The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0049] Choline chloride, lactic acid, and ZnCl2 were mixed in a molar ratio of 1:1:0.2 and heated and stirred at 100°C until the mixture became transparent. The hydrolysis residue A2 was mixed with the mixed catalyst solution in a solid-liquid ratio of 1:20 and stirred at 80°C for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 85.5% and 88.7%, respectively, with purities of 90.3% and 89.2%, respectively.
[0050] Example 3
[0051] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid particles using a pulverizer for storage and later use.
[0052] The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The pressure was set to 1 MPa. The mixture was first pretreated at a low temperature of 120℃ for 30 minutes to remove easily degradable components such as pectin. Then, the inhibitor EDTA (the ratio of Juncao granules to inhibitor was 1:0.02) was added and reacted at a constant temperature of 165℃ for 1 hour. After the reaction was completed, the mixture was filtered to obtain hydrolysate A1 and hydrolysis residue A2.
[0053] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature (40℃) to form hemicellulose powder. The hemicellulose removal rate was 89.9% and the purity was 94.3%.
[0054] The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0055] Choline chloride, formic acid, and ZnCl2 were mixed in a molar ratio of 1:1:0.2 and heated and stirred at 100°C until a transparent solution was obtained. The hydrolysis residue A2 was mixed with the mixed catalyst solution in a solid-liquid ratio of 1:20 and stirred at 80°C for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 83.5% and 83.2%, respectively, with purities of 85.6% and 90.3%, respectively.
[0056] The results showed that citric acid has a higher selectivity for lignin than formic acid and lactic acid, can reduce the degradation of cellulose, and causes less damage to the structure of the removed lignin.
[0057] Comparative Example 1
[0058] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid powder using a pulverizer for storage and later use.
[0059] The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The pressure was set to 1 MPa, and the inhibitor EDTA was added (the ratio of Juncao powder to inhibitor was 1:0.02). The mixture was reacted at a constant temperature of 165°C for 1 hour. After the reaction was completed, the mixture was filtered to separate the hydrolysate A1 and the hydrolysis residue A2.
[0060] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature (40℃) to form hemicellulose powder. The hemicellulose removal rate was 74.9% and the purity was 83.5%.
[0061] The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0062] Choline chloride, citric acid, and ZnCl2 were mixed in a molar ratio of 1:1:0.2 and heated and stirred at 100°C until a transparent solution was obtained. The hydrolysis residue A2 was mixed with the mixed catalyst solution in a solid-liquid ratio of 1:20 and stirred at 80°C for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 87.9% and 89.6%, respectively, with purities of 86.8% and 88.2%, respectively.
[0063] Experimental results show that, compared with Example 1, the removal rate and purity of hemicellulose obtained without low-temperature pretreatment are both reduced.
[0064] Comparative Example 2
[0065] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid particles using a pulverizer for storage and later use.
[0066] The Juncao granules and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The pressure was set to 1 MPa, and the pretreatment was carried out at a low temperature of 120℃ for 30 min to remove easily degradable components such as pectin. Then, the reaction was carried out at a constant temperature of 165℃ for 1 h. After the reaction was completed, the hydrolysate A1 and hydrolysis residue A2 were obtained by filtration.
[0067] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature (40℃) to form hemicellulose powder. The hemicellulose removal rate was 70.9% and the purity was 76.3%.
[0068] The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0069] Choline chloride, citric acid, and ZnCl2 were mixed in a molar ratio of 1:1:0.2 and heated and stirred at 100°C until a transparent solution was obtained. The hydrolysis residue A2 was mixed with the mixed catalyst solution in a solid-liquid ratio of 1:20 and stirred at 80°C for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 85.6% and 86.7%, respectively, with purities of 86.3% and 84.2%, respectively.
[0070] Experimental results show that, compared with Example 1, low-temperature treatment without the addition of inhibitors resulted in a decrease in hemicellulose removal rate and purity, and had a negative impact on the subsequent removal rate and purity of cellulose and lignin.
[0071] Comparative Example 3
[0072] Remove the leaves from the mature Juncao fiber raw material, cut it into sections, wash and dry it, and then crush it into solid particles using a pulverizer for storage and later use.
[0073] The Juncao powder and desalinated water were placed in a hydrolysis pot at a solid-liquid ratio of 1:11. The rotation speed and pressure were set to 1 MPa. The mixture was first pretreated at a low temperature of 120℃ for 30 minutes to remove easily degradable components such as pectin. Then, the inhibitor EDTA (the ratio of Juncao particles to inhibitor was 1:0.02) was added and reacted at a constant temperature of 165℃ for 1 hour. After the reaction was completed, the mixture was filtered to separate the hydrolysate A1 and the hydrolysis residue A2.
[0074] Hydrolysate A1 was centrifuged multiple times, and the supernatant was dried at low temperature to form hemicellulose powder. The hemicellulose removal rate was 89.9% and the purity was 94.3%.
[0075] The hydrolysis residue A2 was washed repeatedly with distilled water and dried to constant weight at 105°C, and then stored in an oven for later use.
[0076] Choline chloride and citric acid were mixed in a 1:1 molar ratio and heated at 100°C with stirring until a transparent solution was obtained. The hydrolysis residue A2 was mixed with the choline chloride and citric acid solution in a 1:20 solid-liquid ratio and reacted at 80°C with stirring for 1.5 hours. After the reaction, the mixture was filtered and washed, yielding cellulose and lignin removal rates of 88.4% and 79.4%, respectively, with purities of 89.3% and 86.2%, respectively.
[0077] Experimental results show that, compared with Example 1, the removal rates of cellulose and lignin were significantly reduced when no catalyst was added.
[0078] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for separating and extracting components from Juncao biomass, characterized in that, The method includes using Juncao grass as raw material, and combining hydrothermal method with mixed catalyst to separate and extract Juncao grass cellulose, hemicellulose and lignin; The mixed catalyst is prepared by mixing choline chloride, acid and catalyst in a ratio of 1:1:0.2 and heating and stirring at 100°C.
2. The method according to claim 1, characterized in that, The acid is lactic acid, oxalic acid, citric acid, malic acid, formic acid, or acetic acid; the catalyst is ZnCl2 or FeCl3.
3. The method according to claim 1, characterized in that, Specifically, the following steps are included: S1. Mix the Juncao granules with desalinated water to carry out a hydrolysis reaction. After the hydrolysis reaction is completed, the products are separated by filtration to obtain hydrolysate and hydrolysis residue respectively. S2. The hydrolysate is centrifuged multiple times, the supernatant is collected, and dried at low temperature to obtain the water-soluble hemicellulose component. S3. After drying, the hydrolysis residue is mixed with the mixed catalyst solution. After the reaction is completed, the residue is filtered and washed to obtain cellulose. The filtrate is then washed with alcohol, water and dried to obtain lignin. The mixed catalyst is prepared by mixing choline chloride, acid and catalyst in a ratio of 1:1:0.2 and heating and stirring at 100°C.
4. The method according to claim 3, characterized in that, In step S1, the mixing ratio of the Juncao granules to the desalinated water is 1:(5-12); the conductivity of the desalinated water is 0.7 μs / cm, pH 7.2, sodium ion concentration is 30 μg / L, and the silicate concentration of the desalinated water is 40 μg / L.
5. The method according to claim 3, characterized in that, The hydrolysis reaction in step S1 includes a low-temperature pretreatment process at 120-140℃ and a high-temperature reaction process at 160-180℃ for 0.5-2 hours after the addition of an inhibitor. The total pressure during the reaction is 1 MPa.
6. The method according to claim 5, characterized in that, The inhibitor is EDTA or glutamic acid-N,N-diacetic acid; the amount of the inhibitor added is 0.01-0.05 times the mass of the Juncao powder.
7. The method according to claim 3, characterized in that, The low-temperature drying conditions described in step S2 are 40°C.
8. The method according to claim 3, characterized in that, The reaction described in step S3 is carried out in a water bath at 70-120°C with stirring for 1-5 hours; the alcohol washing process involves mixing the filtrate with 95% ethanol at a volume ratio of 1:3, letting it stand for 2 hours, then centrifuging it, washing it with water, and freeze-drying it. The resulting solid product is the lignin component.