CN111802556B - Composite impregnated cellulose-based aerogel solid and preparation method thereof - Google Patents
Composite impregnated cellulose-based aerogel solid and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3562—Sugars; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a composite impregnated cellulose-based aerogel solid and a preparation method thereof, wherein the composite impregnated cellulose-based aerogel solid is prepared from 100 parts by weight of crushed nutgrass flatsedge root cellulose aerogel micropore powder and 80-350 parts by weight of pear young leaf extract, the average grain diameter of the crushed nutgrass flatsedge root cellulose aerogel micropore powder is not more than 0.72 mu m, and the volume ratio of micropores is not less than 75%. According to the embodiment of the invention, the composite impregnated cellulose-based aerogel solid can delay the time of the mildew of the feed and reduce the mildew degree of the feed; compared with the prior art, the cost is obviously reduced, and the mildew-proof effect is equivalent, so that the chemical mildew-proof agent and the composite mildew-proof agent are effectively replaced, and the environment-friendly and non-toxic effects are realized.
Description
Technical Field
The invention belongs to the technical field of feeds, and particularly relates to a composite impregnated cellulose-based aerogel solid and a preparation method thereof.
Background
The feed mildew preventive is a common feed additive and is used for inhibiting the generation of mould and toxin, preventing the loss of nutrient components of the feed during the storage period, slowing down the mildew of the feed and prolonging the storage time of the feed. The existing feed mildew-proof additive mainly comprises three types of chemical mildew-proof agents, composite mildew-proof agents and Chinese herbal medicine mildew-proof agents. The chemical mildew preventive mainly comprises propionic acid and salts thereof, sodium diacetate, sorbic acid and the like. The chemical mildew preventive has the defect that the mildew preventive has the mildew preventive effect inversely proportional to corrosiveness and is easy to produce toxic and side effects. The compound mildew preventive is prepared by mixing a plurality of organic acid or organic acid salt mildew preventive according to a certain proportion, and the mildew preventive has better mildew preventive effect than a single chemical mildew preventive, but the compound mildew preventive is easy to damage the whole nutrition level of the feed. The mildew-proof effect of the Chinese herbal medicine mildew inhibitor is realized through bacteriostasis growth and propagation, has no residue, no drug resistance and no toxic or side effect, and is an important development direction of feed mildew-proof additives. In practical application, the Chinese herbal medicine feed mildew-proof additive has the following defects: 1) The self stability is not high, and the storage is inconvenient because the self stability is easy to be influenced by light, heat, moisture and the like in the application process; 2) The slow release effect is not obvious, and the mildew-proof aging is not durable; 3) The Chinese herbal medicines are various, and the proper raw materials and preparation process are adopted, so that the raw materials and manufacturing cost are reduced, the cost performance is improved, and the continuous intensive research is required.
The crushed cyperus rotundus grows in various places almost nationwide, especially in farmlands, and damages the growth of rice, soybean, cotton, vegetables and fruit trees, and is a harmful plant. However, the root of the crushed nutgrass galingale rhizome is rich in specific total alkaloids, so that the crushed nutgrass galingale rhizome has a bacteriostatic action, how to convert the crushed nutgrass galingale rhizome with low cost and rich sources into waste into valuable substances is worthy of attention and research, and how to ensure the stability of the crushed nutgrass galingale rhizome and simultaneously ensure the slow release effect and finally obtain the reasonable mildew-proof and bacteriostatic effects is a difficulty in preparation.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a composite impregnated cellulose-based aerogel solid and a preparation method thereof, and the main points of the invention are as follows:
according to one aspect of the invention, the composite impregnated cellulose-based aerogel solid is prepared from 100 parts by weight of crushed nutgrass galingale root cellulose aerogel micropore powder and 80-350 parts by weight of young pear leaf extract according to the weight part ratio, wherein the average particle size of the crushed nutgrass galingale root cellulose aerogel micropore powder is not more than 0.72 mu m, and the volume ratio of micropores is not less than 75%.
According to another aspect of the invention, a method of preparing a composite coated cellulose-based aerogel solid, the method comprising:
1. extraction of cellulose from root of Cyperus rotundus
1) Pretreatment: shearing, drying, crushing and sieving the cleaned crushed cyperus rotundus roots to obtain 50-mu m crushed cyperus rotundus root powder;
2) Acidifying pretreatment: soaking the crushed nutgrass galingale rhizome powder for 60min at 35 ℃ by adopting 0.1mol/L oxalic acid solution according to a solid-liquid ratio of 1:30, and drying after suction filtration to obtain a first intermediate product;
3) Alkalizing leaching: leaching the first intermediate product with 0.2mol/L sodium hydroxide solution at 90 ℃ for 80min according to a solid-liquid ratio of 1:15, and drying after suction filtration to obtain a second intermediate product;
4) Purifying: the second intermediate product is subjected to constant temperature water bath at 80 ℃ for 60min by adopting sodium hypochlorite solution with the concentration of 0.2mol/L according to the solid-liquid ratio of 1:10; washing with absolute ethanol to neutrality, and vacuum drying at 60deg.C to obtain rhizoma Cyperi.
2. Preparation of crushed nutgrass flatsedge root cellulose aerogel microporous powder
1) Preparation of cellulose aerogel precursor at root of rhizoma cyperi
Activating cellulose at the roots of the crushed nutgrass galingale rhizome: adding 100 parts by weight of crushed nutgrass flatsedge root cellulose into 280-400 parts by weight of N, N-dimethylacetamide solvent according to the weight ratio, and stirring for 20min in a constant-temperature water bath at 100 ℃ to obtain an activated nutgrass flatsedge root cellulose solution;
dissolving cellulose at the root of the nutgrass flatsedge: cooling the activated cyperus rotundus root cellulose solution to 70 ℃, adding 15 parts by weight of sodium chloride, and stirring at constant temperature for 2 hours to obtain an intermediate cellulose solution;
microfibrillating treatment: carrying out microfibrillation treatment on the intermediate cellulose solution under the ice water bath condition by adopting a high-frequency ultrasonic cell disruption instrument to obtain microfibrillated sol;
gel precursor preparation: and (3) standing the microfibrillated sol at 10+/-1 ℃ for 8 hours, and fully washing with absolute ethyl alcohol to obtain the precursor of the cellulose aerogel at the root of the cyperus rotundus.
2) Crosslinking treatment
Preparing a crosslinking initiation solution from acetic acid and sodium acetate solution according to the mass ratio of 4:1; and (3) fully soaking the precursor of the cellulose aerogel of the crushed nutgrass flatsedge root by adopting a crosslinking initiation solution at the temperature of 45+/-2 ℃ for 5 hours to obtain the crosslinked and reinforced cellulose gel of the crushed nutgrass flatsedge root.
3) Purification treatment
Immersing the crosslinked and reinforced crushed cyperus rotundus root cellulose gel into a supercritical purifier storing absolute ethyl alcohol, and purifying.
4) Shaping treatment
And (3) carrying out shaping treatment on the gel subjected to purification treatment to obtain the crushed nutgrass flatsedge root cellulose aerogel microporous powder.
3. Preparation of extractive solution of young leaves of fructus Pyri
Adding the young leaves of the pears into absolute ethyl alcohol according to the solid-to-liquid ratio of 1:15, carrying out ultrasonic extraction for 80min, filtering, and carrying out drying sterilization at 121 ℃ for 20s to obtain the young leaves of the pears.
4. Preparation of composite impregnated cellulose-based aerogel solids
The weight ratio of the components is as follows: 100 parts by weight of crushed cyperus rotundus root cellulose aerogel microporous powder and 80-350 parts by weight of pear young leaf extract;
adding the young leaf extract of the wood pears into absolute ethyl alcohol, fully stirring and dissolving in a sealed reaction kettle, adding crushed nutgrass galingale root cellulose aerogel microporous powder, setting the pressure in the sealed reaction kettle to be 5MPa, electromagnetically stirring for 100min at the temperature of 60 ℃ and discharging the mixture out of the reaction kettle, and evaporating and drying to obtain the composite impregnated cellulose-based aerogel solid.
According to an exemplary embodiment of the present invention, the ultrasonic frequency is 15.5-17.5kHz, the ultrasonic time is 10min, and the pulse interval is 5s during the microfibrillation treatment.
According to an exemplary embodiment of the present invention, the concentration of acetic acid is 0.1mol/L and the concentration of sodium acetate solution is 0.15mol/L at the time of the crosslinking treatment.
According to an exemplary embodiment of the present invention, the temperature in the supercritical purifier is-5 ℃, the pressure is 5.2MPa, and the purification medium is liquid CO 2 。
According to an exemplary embodiment of the present invention, the molding temperature is 105 ℃ and the molding time is 2h to 6.5h during the molding process.
The invention relates to a method for preparing a composite impregnated cellulose-based aerogel solid by extracting cellulose at the root of a crushed nutgrass galingale rhizome, preparing cellulose aerogel microporous powder at the root of the crushed nutgrass galingale rhizome and preparing a young leaf extract of a wood pear. According to the embodiment of the invention, the composite impregnated cellulose-based aerogel solid can delay the time of the mildew of the feed and reduce the mildew degree of the feed; compared with the prior art, the cost is obviously reduced, and the mildew-proof effect is equivalent, so that the chemical mildew-proof agent and the composite mildew-proof agent are effectively replaced, and the environment-friendly and non-toxic effects are realized.
Drawings
FIG. 1 is a graph of MIC values for a composite coated cellulose-based aerogel solids sample in comparison to a prior art sample according to an embodiment of the present invention.
Detailed Description
In order to make the technical scheme and advantages of the present invention more clear, the present invention will be described in further detail by the following several specific examples. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples:
preparation of composite impregnated cellulose-based aerogel solids
1. Extraction of cellulose from root of Cyperus rotundus
1) Pretreatment: shearing, drying, crushing and sieving the cleaned crushed cyperus rotundus roots to obtain 50-mu m crushed cyperus rotundus root powder;
2) Acidifying pretreatment: soaking the crushed nutgrass galingale rhizome powder for 60min at 35 ℃ by adopting 0.1mol/L oxalic acid solution according to a solid-liquid ratio of 1:30, and drying after suction filtration to obtain a first intermediate product;
3) Alkalizing leaching: leaching the first intermediate product with 0.2mol/L sodium hydroxide solution at 90 ℃ for 80min according to a solid-liquid ratio of 1:15, and drying after suction filtration to obtain a second intermediate product;
4) Purifying: the second intermediate product is subjected to constant temperature water bath at 80 ℃ for 60min by adopting sodium hypochlorite solution with the concentration of 0.2mol/L according to the solid-liquid ratio of 1:10; washing with deionized water and absolute ethanol to neutrality, and vacuum drying at 60deg.C to obtain rhizoma Cyperi.
2. Preparation of crushed nutgrass flatsedge root cellulose aerogel microporous powder
1) Preparation of cellulose aerogel precursor at root of rhizoma cyperi
Activating cellulose at the roots of the crushed nutgrass galingale rhizome: adding 100 parts by weight of crushed nutgrass flatsedge root cellulose into 280-400 parts by weight of N, N-dimethylacetamide solvent according to the weight ratio, and stirring for 20min in a constant-temperature water bath at 100 ℃ to obtain an activated nutgrass flatsedge root cellulose solution;
dissolving cellulose at the root of the nutgrass flatsedge: cooling the activated cyperus rotundus root cellulose solution to 70 ℃, adding 15 parts by weight of sodium chloride, and stirring at constant temperature for 2 hours to obtain an intermediate cellulose solution;
microfibrillating treatment: carrying out microfibrillation treatment on the intermediate cellulose solution under the ice water bath condition by adopting a high-frequency ultrasonic cell disruption instrument, wherein the ultrasonic frequency is 15.5-17.5kHz, the ultrasonic time is 10min, and the pulse interval is 5s, so as to obtain microfibrillated sol;
gel precursor preparation: and (3) standing the microfibrillated sol at 10+/-1 ℃ for 8 hours, and fully washing with absolute ethyl alcohol to obtain the precursor of the cellulose aerogel at the root of the cyperus rotundus.
2) Crosslinking treatment
Preparing a crosslinking initiation solution from 0.1mol/L acetic acid and 0.15mol/L sodium acetate solution according to the mass ratio of 4:1; and (3) fully soaking the precursor of the cellulose aerogel of the crushed nutgrass flatsedge root by adopting a crosslinking initiation solution at the temperature of 45+/-2 ℃ for 5 hours to obtain the crosslinked and reinforced cellulose gel of the crushed nutgrass flatsedge root.
3) Purification treatment
Immersing crosslinked and reinforced cellulose gel at the root of Cyperus rotundus L in supercritical purifier with anhydrous ethanol at-5deg.C under pressureThe force is 5.2MPa, and the purification medium is liquid CO 2 And (5) purifying.
4) Shaping treatment
And (3) carrying out shaping treatment on the gel subjected to the purification treatment, wherein the shaping temperature is 105 ℃, and the shaping time is 2-6.5 h, so as to obtain the crushed cyperus root cellulose aerogel microporous powder.
3. Preparation of extractive solution of young leaves of fructus Pyri
Adding the young leaves of the pears into absolute ethyl alcohol according to the solid-to-liquid ratio of 1:15, carrying out ultrasonic extraction for 80min, filtering, and carrying out drying sterilization at 121 ℃ for 20s to obtain the young leaves of the pears.
4. Preparation of composite impregnated cellulose-based aerogel solids
The weight ratio of the components is as follows: 100 parts by weight of crushed cyperus rotundus root cellulose aerogel microporous powder and 80-350 parts by weight of pear young leaf extract;
adding the young leaf extract of the wood pears into absolute ethyl alcohol, fully stirring and dissolving in a sealed reaction kettle, adding crushed nutgrass galingale root cellulose aerogel microporous powder, setting the pressure in the sealed reaction kettle to be 5MPa, electromagnetically stirring for 100min at the temperature of 60 ℃ and discharging the mixture out of the reaction kettle, and evaporating and drying to obtain the composite impregnated cellulose-based aerogel solid.
A plurality of groups of tests are prepared according to the preparation method, wherein the sample groups are respectively numbered as T1, T2, T3, T4 and T5, and the proportions of the tests in each group are shown in Table 1.
TABLE 1
Detection of specifications of crushed nutgrass galingale root cellulose aerogel microporous powder
According to the technical scheme of preparing the composite impregnated cellulose-based aerogel solid in example 1, after the molding treatment, a crushed nutgrass galingale root cellulose aerogel microporous powder sample group is obtained, wherein the sample groups are respectively numbered as S1, S2, S3, S4 and S5.
The average particle size of the crushed cyperus root cellulose aerogel microporous powder is measured according to ASTM E2980-2014, standard test method for evaluating average particle size of powder by air permeability; measuring the volume ratio of micropores in the crushed nutgrass flatsedge root cellulose aerogel microporous powder according to GB/T21650-2008 mercury compression method and gas adsorption method for measuring the pore size distribution and the porosity of a solid material; the measurement results are shown in Table 2.
TABLE 2
Compound impregnated cellulose-based aerogel solid mildew-proof effect test
The compound impregnated cellulose-based aerogel solid prepared in the embodiment of the application is used as a common feed for verifying the mildew-proof effect, and the formula of the feed for the test is as follows: 67% of corn, 25% of bean pulp, 6% of pre-powder and 2% of soybean oil;
the composite impregnated cellulose-based aerogel solid prepared in the embodiment of the application is used as a mildew-proof additive and added into test feed, and the sample numbers are respectively F1, F2, F3, F4 and F5, and the adding proportion is 0.3%. Sodium diacetate, citric acid and calcium propionate are respectively taken as mildew-proof additives and added into test feed in a proportion of 0.3 percent to form control groups D1, D2 and D3; the test feed without the addition of the mildew preventive additive was control group D4.
After being uniformly mixed, each group of samples are placed in a constant temperature incubator with the temperature of 30 ℃ and the relative humidity of 90%, 5 repetitions are set for each treatment, and sampling analysis is carried out on days 1, 2, 4, 6, 8, 10, 15 and 30 respectively; sensory evaluation was performed on each sample group by observing the odor, caking and mildew of the sample group, evaluation criteria: whether the smell has rancid smell, mould smell and other peculiar smell; whether the form viscosity is increased, whether the feed is agglomerated, and whether the feed is used for growing insects; the evaluation results are shown in Table 3 (the more "+" shows more serious mildewing).
TABLE 3 Table 3
As can be seen from table 3, the composite impregnated cellulose-based aerogel solid prepared in the embodiment of the present application can delay the time of mildew of the feed and can reduce the mildew degree of the feed; compared with the prior art, the mildew-proof effect is equivalent under the same test condition.
Compound immersed cellulose-based aerogel solid antibacterial test
Test indicator bacteria: fusarium moniliforme is an indicator bacterium.
Test medium: 1% of tryptone, 0.5% of yeast extract powder, 2% of glucose and pH 6.8.
The test method comprises the following steps: taking 250mL triangular bottles, adding 50mL of culture medium into each bottle, and sterilizing at high temperature; cleaning fusarium moniliforme spores by adopting sterile physiological saline, and adding 0.5mL of spore water into each bottle of culture medium; the composite impregnated cellulose-based aerogel solid prepared in the embodiment of the application is used as a mildew-proof additive and added into a culture medium, and sample components are respectively numbered as T1, T2, T3, T4 and T5. Sodium diacetate, citric acid and calcium propionate are respectively taken as mildew-proof additives and added into a culture medium to form control groups d1, d2 and d3; the medium without the addition of the mildew-proof additive was control d4. And culturing for 20 hours at a constant temperature under the test condition of 28 ℃ and 200r/min, and observing the test result, wherein each additive concentration without mould growth is the MIC value (mg/mL) of the minimum inhibitory concentration.
TABLE 4 Table 4
As can be seen from table 4 and fig. 1, the composite impregnated cellulose-based aerogel solid prepared in the examples of the present application has antibacterial and mildew-proof effects; compared with the prior art, under the same test condition, the antibacterial and mildew-proof effects are equivalent.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (4)
1. A method of preparing a composite coated cellulose-based aerogel solid, the method comprising:
1. extraction of cellulose from root of Cyperus rotundus
1) Pretreatment: shearing, drying, crushing and sieving the cleaned crushed cyperus rotundus roots to obtain 50-mu m crushed cyperus rotundus root powder;
2) Acidifying pretreatment: soaking the crushed nutgrass galingale rhizome powder for 60min at 35 ℃ by adopting 0.1mol/L oxalic acid solution according to a solid-liquid ratio of 1:30, and drying after suction filtration to obtain a first intermediate product;
3) Alkalizing leaching: leaching the first intermediate product with 0.2mol/L sodium hydroxide solution at 90 ℃ for 80min according to a solid-liquid ratio of 1:15, and drying after suction filtration to obtain a second intermediate product;
4) Purifying: the second intermediate product is subjected to constant temperature water bath at 80 ℃ for 60min by adopting sodium hypochlorite solution with the concentration of 0.2mol/L according to the solid-liquid ratio of 1:10; washing with absolute ethanol to neutrality, and vacuum drying at 60deg.C to obtain rhizoma Cyperi preparata root cellulose;
2. preparation of crushed nutgrass flatsedge root cellulose aerogel microporous powder
1) Preparation of cellulose aerogel precursor at root of rhizoma cyperi
Activating cellulose at the roots of the crushed nutgrass galingale rhizome: adding 100 parts by weight of crushed nutgrass flatsedge root cellulose into 280-400 parts by weight of N, N-dimethylacetamide solvent according to the weight ratio, and stirring for 20min in a constant-temperature water bath at 100 ℃ to obtain an activated nutgrass flatsedge root cellulose solution;
dissolving cellulose at the root of the nutgrass flatsedge: cooling the activated cyperus rotundus root cellulose solution to 70 ℃, adding 15 parts by weight of sodium chloride, and stirring at constant temperature for 2 hours to obtain an intermediate cellulose solution;
microfibrillating treatment: carrying out microfibrillation treatment on the intermediate cellulose solution under the ice water bath condition by adopting a high-frequency ultrasonic cell disruption instrument to obtain microfibrillated sol;
gel precursor preparation: standing the microfibrillated sol at 10+/-1 ℃ for 8 hours, and fully washing the microfibrillated sol by using absolute ethyl alcohol to obtain a precursor of the cellulose aerogel at the root of the cyperus rotundus;
2) Crosslinking treatment
Preparing a crosslinking initiation solution from acetic acid and sodium acetate solution according to the mass ratio of 4:1; fully soaking the precursor of the cellulose aerogel of the root parts of the crushed nutgrass flatsedge by adopting a crosslinking initiation solution at the temperature of 45+/-2 ℃ for 5 hours to obtain crosslinked and reinforced cellulose gel of the root parts of the crushed nutgrass flatsedge; during the crosslinking treatment, the concentration of acetic acid is 0.1mol/L, and the concentration of sodium acetate solution is 0.15mol/L;
3) Purification treatment
Immersing the crosslinked and reinforced crushed cyperus rotundus root cellulose gel into a supercritical purifier storing absolute ethyl alcohol for purification treatment;
4) Shaping treatment
Shaping the gel subjected to purification treatment to obtain crushed nutgrass flatsedge root cellulose aerogel microporous powder; the average grain diameter of the cellulose aerogel micropore powder at the root of the nutgrass flatsedge is not more than 0.72 mu m, and the volume ratio of micropores is not less than 75%;
3. preparation of extractive solution of young leaves of fructus Pyri
Adding the young leaves of the pears into absolute ethyl alcohol according to a solid-to-liquid ratio of 1:15, performing ultrasonic extraction for 80min, filtering, and performing drying and sterilization treatment at 121 ℃ for 20s to obtain young leaf extracts of the pears;
4. preparation of composite impregnated cellulose-based aerogel solids
The weight ratio of the components is as follows: 100 parts by weight of crushed cyperus rotundus root cellulose aerogel microporous powder and 80-350 parts by weight of pear young leaf extract;
adding the young leaf extract of the wood pears into absolute ethyl alcohol, fully stirring and dissolving in a sealed reaction kettle, adding crushed nutgrass galingale root cellulose aerogel microporous powder, setting the pressure in the sealed reaction kettle to be 5MPa, electromagnetically stirring for 100min at the temperature of 60 ℃ and discharging the mixture out of the reaction kettle, and evaporating and drying to obtain the composite impregnated cellulose-based aerogel solid.
2. The method according to claim 1, wherein the ultrasonic frequency is 15.5-17.5kHz, the ultrasonic time is 10min, and the pulse interval is 5s.
3. The method according to claim 1, wherein the supercritical purifier is operated at a temperature of-5deg.C and a pressure of 5.2MPa, and the purification medium is liquid CO 2 。
4. The method according to claim 1, wherein the molding temperature is 105 ℃ and the molding time is 2h to 6.5h.
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