CN110787774A - Chitosan-manganese dioxide composite adsorption material and preparation method thereof - Google Patents
Chitosan-manganese dioxide composite adsorption material and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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Abstract
The invention discloses a preparation method of a chitosan-manganese dioxide composite adsorption material, which comprises the following steps: step 1, preparing a redox reaction base solution: fully dissolving potassium permanganate powder in distilled water, adding oleic acid into the solution, and stirring to form O/W emulsion; step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature; step 3; cleaning: washing the soaked chitosan degradable fiber with absolute ethyl alcohol to remove unreacted oleic acid, and washing with distilled water to remove residual ethyl alcohol; and 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours. The invention also discloses a chitosan-manganese dioxide composite adsorbing material. The invention realizes the preparation of the chitosan composite material at room temperature, so that the chitosan purification base material can be effectively compounded with other materials without adding a binder.
Description
Technical Field
The invention belongs to the technical field of material preparation and application, relates to a chitosan composite material and a preparation method thereof, and particularly relates to a chitosan-manganese dioxide composite adsorption material and a preparation method thereof.
Background
At present, along with the economic rapid development, the formaldehyde pollution problem brought by building materials and indoor furniture materials is increasingly serious, and the formaldehyde in the air is removed in a mode of combining photocatalysis and adsorption at home and abroad, so that the adsorption material has the following problems: the selectivity is poor, and the adsorption is easy to saturate; poor recycling performance and high use cost. The chitosan serving as a degradable organic high polymer material has high antibacterial property, biological functionality and compatibility, is an environment-friendly bio-based material, contains a large amount of amino and hydroxyl on the surface, and has excellent adsorption performance.
Because the chitosan adsorbs formaldehyde, belonging to chemical adsorption, the adsorption process is slow, and the pure chitosan has limited formaldehyde gas purification capacity and rate, and the adsorption performance of the chitosan is improved by frequently modifying the chitosan. Most of chitosan adsorption materials on the market are granular, but loose chitosan granules or powder are difficult to recover and regenerate after being adsorbed to saturation, and the mechanical extrusion in the forming process can cause the damage of the structure, the stacking density is increased, and the adsorption quantity is reduced. At present, the patent technologies related to the chitosan composite fiber with the air purification function are few, so a new technology for preparing the chitosan composite adsorption material needs to be developed to meet the requirements of the fiber manufacturing technology and the human living environment field.
Disclosure of Invention
Aiming at the defects and the shortcomings of the chitosan adsorption material, the invention prepares the dioxide and chitosan composite material by utilizing the chelation of chitosan to transition metal, and provides the chitosan-manganese dioxide composite adsorption material with improved formaldehyde purification effect and the preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems in the prior art is as follows: a preparation method of a chitosan-manganese dioxide composite adsorption material comprises the following steps:
step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature;
step 3; cleaning: washing the soaked chitosan degradable fiber with absolute ethyl alcohol to remove unreacted oleic acid, and washing with distilled water to remove residual ethyl alcohol;
and 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours.
Further, in step 1, the specific method for preparing the redox reaction base solution is as follows: at room temperature, dispersing potassium permanganate powder in distilled water, and stirring for 20-30 minutes at a stirring speed of 800 revolutions per minute by using a magnetic stirrer to completely dissolve potassium permanganate; and dropwise adding oleic acid into the solution, and stirring for 4-6 minutes at the stirring speed of 800 revolutions per minute by adopting a magnetic stirrer to form O/W emulsion.
Further, the redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 0.5-1 part of potassium permanganate and 4.45-8.9 parts of oleic acid.
Further, the redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 0.5 part of potassium permanganate and 8.9 parts of oleic acid.
Further, the mass ratio of the chitosan degradation fiber to the redox reaction base solution is 1: 100 to 130.
Further, the emulsion after mixing potassium permanganate and oleic acid is subjected to redox reaction, and manganese dioxide generated by the reaction is in-situ deposited on the surface of the chitosan degradation fiber.
Further, the chitosan degradable fiber adopts chitosan needle-punched cloth.
The invention also provides a chitosan-manganese dioxide composite adsorbing material which is prepared by the preparation method of the chitosan-manganese dioxide composite adsorbing material.
The invention has the advantages and positive effects that: compared with the prior art, the invention has the following beneficial effects:
(1) the invention realizes the preparation of the chitosan composite material under the room temperature condition, so that the chitosan purification base material can be effectively compounded with other materials without adding a binder.
(2) The invention realizes the in-situ loading directly by potassium permanganate; the process of independent load is omitted, and the energy consumption and the production cost are reduced.
(3) The chitosan is used as a base material, and can effectively sterilize and inhibit bacteria. The loading process can generate new defects, cavities and the like on the surface of the material, so that a new adsorption space is provided, and the material has longer service life compared with the traditional material mainly based on physical adsorption. The fibrous design ensures that the air permeability of the invention is good, and the filtering material has small air passing resistance while ensuring the filtering effect.
Drawings
FIG. 1 is an SEM image at 1500 times magnification of a chitosan needle punched cloth used in the present invention;
FIG. 2 is an SEM image of chitosan-manganese dioxide composite adsorbing material prepared in the invention, which is magnified 2000 times;
FIG. 3 is an SEM image of portion A of FIG. 2 at 10000 times magnification;
FIG. 4 is a comparison of formaldehyde purification effect of chitosan and chitosan-manganese dioxide composite adsorbing material (20cm × 20 cm);
FIG. 5 is a schematic diagram showing the comparison of the resistances of chitosan and chitosan-manganese dioxide composite adsorbing materials at different filtration rates.
Detailed Description
For further understanding of the contents, features and effects of the present invention, the following embodiments are enumerated in conjunction with the accompanying drawings, and the following detailed description is given:
the preparation method of the chitosan-manganese dioxide composite adsorbing material, in example 1, comprises the following steps:
The redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 0.5 part of potassium permanganate and 4.45 parts of oleic acid.
This corresponds to dissolving 0.5g of potassium permanganate powder in 500ml of distilled water, then dropping about 5ml of oleic acid, and sufficiently stirring to form a redox reaction base solution.
The specific method for preparing the redox reaction base solution may be as follows: at room temperature, potassium permanganate powder is taken to be dispersed in distilled water, and a magnetic stirrer can be adopted to stir at the stirring speed of 800 revolutions per minute for 30 minutes, so that potassium permanganate is completely dissolved; oleic acid was then added dropwise to the solution, which was stirred for 6 minutes using a magnetic stirrer at a stirring speed of 800 revolutions per minute to form an O/W emulsion.
Step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature; wherein, the mass ratio of the chitosan degradation fiber to the redox reaction base solution can be 1: 100. the chitosan degradable fiber can adopt chitosan needle-punched cloth. The base liquid for the redox reaction prepared according to the proportion can be injected into a rectangular container, and the chitosan needle punched cloth (95 g/square meter) can be immersed into the mixed liquid to ensure that the base liquid can completely permeate the adsorption fibers.
The emulsion after the potassium permanganate and the oleic acid are mixed is subjected to oxidation-reduction reaction, and manganese dioxide generated by the reaction can be in-situ deposited on the surface of the chitosan degradation fiber.
Step 3; cleaning: washing the soaked chitosan degradable fiber with absolute ethyl alcohol to remove unreacted oleic acid, and washing with distilled water to remove residual ethyl alcohol;
the soaked chitosan degradable fibers become manganese dioxide-loaded chitosan needle-punched cloth, the chitosan needle-punched cloth is placed in absolute ethyl alcohol for alcohol washing treatment, the alcohol washing treatment time can be 10min each time, alcohol washing can be carried out for 3 times, then distilled water is used for washing, washing can be carried out for 3 times, and residual absolute ethyl alcohol is removed.
And 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours. And then taking out the dried manganese dioxide-loaded chitosan needle-punched cloth forming body to prepare the chitosan-manganese dioxide composite adsorbing material. The loading capacity of manganese dioxide in the prepared chitosan composite adsorbing material is measured to be 0.51mg/cm2。
The chitosan-manganese dioxide composite adsorbing material is prepared according to the preparation method, and the formaldehyde gas purifying capacity is as follows: the amount of formaldehyde adsorbed at 25 ℃ was 0.82 mg/g.
Embodiment 2 of a method for preparing a chitosan-manganese dioxide composite adsorbing material comprises the following steps:
The redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 0.75 part of potassium permanganate and 6.675 parts of oleic acid.
This corresponds to dissolving 0.75g of potassium permanganate powder in 500ml of distilled water, adding about 7.5ml of oleic acid dropwise thereto, and sufficiently stirring the resulting solution to form a redox reaction base solution.
The specific method for preparing the redox reaction base solution may be as follows: at room temperature, potassium permanganate powder is taken to be dispersed in distilled water, and a magnetic stirrer can be adopted to stir at the stirring speed of 800 revolutions per minute for 30 minutes, so that potassium permanganate is completely dissolved; oleic acid was then added dropwise to the solution, which was stirred for 6 minutes using a magnetic stirrer at a stirring speed of 800 revolutions per minute to form an O/W emulsion.
Step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature; wherein, the mass ratio of the chitosan degradation fiber to the redox reaction base solution can be 1: 115. the chitosan degradable fiber can adopt chitosan needle-punched cloth. The base liquid for the redox reaction prepared according to the proportion can be injected into a rectangular container, and the chitosan needle punched cloth (95 g/square meter) can be immersed into the mixed liquid to ensure that the base liquid can completely permeate the adsorption fibers.
The emulsion after the potassium permanganate and the oleic acid are mixed is subjected to oxidation-reduction reaction, and manganese dioxide generated by the reaction can be in-situ deposited on the surface of the chitosan degradation fiber.
Step 3; cleaning: washing the soaked chitosan degraded fiber with absolute ethanol for 3 times to remove unreacted oleic acid, and washing with distilled water for 3 times to remove residual ethanol;
the soaked chitosan degradable fibers become manganese dioxide-loaded chitosan needle-punched cloth, the chitosan needle-punched cloth is placed in absolute ethyl alcohol for alcohol washing treatment, the alcohol washing treatment time can be 10min each time, alcohol washing can be carried out for 3 times, then distilled water is used for washing, washing can be carried out for 3 times, and residual absolute ethyl alcohol is removed.
And 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours. And then taking out the dried manganese dioxide-loaded chitosan needle-punched cloth forming body to prepare the chitosan-manganese dioxide composite adsorbing material. The loading capacity of manganese dioxide in the prepared chitosan composite adsorbing material is measured to be 1.3mg/cm2。
The chitosan-manganese dioxide composite adsorbing material prepared by the preparation method has the following formaldehyde gas purifying capacity and formaldehyde gas purifying rate: the amount of formaldehyde adsorbed at 25 ℃ was 1.05 mg/g.
Embodiment 3 of a method for preparing a chitosan-manganese dioxide composite adsorbing material comprises the following steps:
The redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 1 part of potassium permanganate and 8.9 parts of oleic acid.
This corresponds to dissolving 1g of potassium permanganate powder in 500ml of distilled water, then dropping 10ml of oleic acid, and stirring them thoroughly to form a redox reaction base solution.
The specific method for preparing the redox reaction base solution may be as follows: at room temperature, potassium permanganate powder is taken to be dispersed in distilled water, and a magnetic stirrer can be adopted to stir at the stirring speed of 800 revolutions per minute for 30 minutes, so that potassium permanganate is completely dissolved; oleic acid was then added dropwise to the solution, which was stirred for 6 minutes using a magnetic stirrer at a stirring speed of 800 revolutions per minute to form an O/W emulsion.
Step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature; wherein, the mass ratio of the chitosan degradation fiber to the redox reaction base solution can be 1: 130. the chitosan degradable fiber can adopt chitosan needle-punched cloth. The base liquid for the redox reaction prepared according to the proportion can be injected into a rectangular container, and the chitosan needle punched cloth (95 g/square meter) can be immersed into the mixed liquid to ensure that the base liquid can completely permeate the adsorption fibers.
The emulsion after the potassium permanganate and the oleic acid are mixed is subjected to oxidation-reduction reaction, and manganese dioxide generated by the reaction can be in-situ deposited on the surface of the chitosan degradation fiber.
Step 3, cleaning: washing the soaked chitosan degraded fiber with absolute ethanol for 3 times to remove unreacted oleic acid, and washing with distilled water for 3 times to remove residual ethanol;
the soaked chitosan degradable fibers become manganese dioxide-loaded chitosan needle-punched cloth, the chitosan needle-punched cloth is placed in absolute ethyl alcohol for alcohol washing treatment, the alcohol washing treatment time can be 10min each time, alcohol washing can be carried out for 3 times, then distilled water is used for washing, washing can be carried out for 3 times, and residual absolute ethyl alcohol is removed.
And 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours. And then taking out the dried manganese dioxide-loaded chitosan needle-punched cloth forming body to prepare the chitosan-manganese dioxide composite adsorbing material. The loading capacity of manganese dioxide in the prepared chitosan composite adsorbing material is measured to be 2.55mg/cm2。
The chitosan-manganese dioxide composite adsorbing material prepared by the preparation method has the following formaldehyde gas purifying capacity and formaldehyde gas purifying rate: the amount of formaldehyde adsorbed at 25 ℃ was 1.03 mg/g.
Embodiment 4 of a method for preparing a chitosan-manganese dioxide composite adsorbing material comprises the following steps:
The redox reaction base solution is prepared from the following raw materials in parts by weight: 500 parts of distilled water, 0.8 part of potassium permanganate and 7.12 parts of oleic acid.
This corresponds to dissolving 0.8g of potassium permanganate powder in 500ml of distilled water, then dropping 8ml of oleic acid, and sufficiently stirring to form a redox reaction base solution.
The specific method for preparing the redox reaction base solution may be as follows: at room temperature, potassium permanganate powder is taken to be dispersed in distilled water, and a magnetic stirrer can be adopted to stir at the stirring speed of 800 revolutions per minute for 20-30 minutes, so that potassium permanganate is completely dissolved; and dropwise adding oleic acid into the solution, and stirring for 4-6 minutes at the stirring speed of 800 revolutions per minute by adopting a magnetic stirrer to form O/W emulsion.
Step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature; wherein, the mass ratio of the chitosan degradation fiber to the redox reaction base solution can be 1: 110. the chitosan degradable fiber can adopt chitosan needle-punched cloth. The base liquid for the redox reaction prepared according to the proportion can be injected into a rectangular container, and the chitosan needle punched cloth (95 g/square meter) can be immersed into the mixed liquid to ensure that the base liquid can completely permeate the adsorption fibers.
The emulsion after the potassium permanganate and the oleic acid are mixed is subjected to oxidation-reduction reaction, and manganese dioxide generated by the reaction can be in-situ deposited on the surface of the chitosan degradation fiber.
Step 3; cleaning: washing the soaked chitosan degraded fiber with absolute ethanol for 3 times to remove unreacted oleic acid, and washing with distilled water for 3 times to remove residual ethanol;
the soaked chitosan degradable fibers become manganese dioxide-loaded chitosan needle-punched cloth, the chitosan needle-punched cloth is placed in absolute ethyl alcohol for alcohol washing treatment, the alcohol washing treatment time can be 10min each time, alcohol washing can be carried out for 3 times, then distilled water is used for washing, washing can be carried out for 3 times, and residual absolute ethyl alcohol is removed.
And 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours. And then taking out the dried manganese dioxide-loaded chitosan needle-punched cloth forming body to prepare the chitosan-manganese dioxide composite adsorbing material. The loading amount of manganese dioxide in the prepared chitosan composite adsorbing material is measured to be 1.71mg/cm2。
The chitosan-manganese dioxide composite adsorbing material prepared by the preparation method has the following formaldehyde gas purifying capacity and formaldehyde gas purifying rate: the amount of formaldehyde adsorbed at 25 ℃ was 1.15 mg/g.
Fig. 1 is an SEM image of a chitosan needle punched cloth used in the present invention at 1500 times magnification.
Fig. 2 is an SEM image of a chitosan-manganese dioxide composite adsorbent material according to the present invention, which is obtained by the preparation method of the above-described 4 th example, at 2000 times magnification. Fig. 3 is an SEM image of part a of fig. 2, partially magnified 10000 times.
At the ambient temperature of 23 +/-2 ℃ and the ambient relative humidity of 50 +/-10 percent at 30m3In a closed environment cabin, the sterilization experimental results of the chitosan-manganese dioxide composite adsorbing material prepared by the preparation method of the chitosan-manganese dioxide composite adsorbing material described in the above examples 1, 2 and 3 are shown in the following table 1, wherein:
test No. 1 is a chitosan-manganese dioxide composite adsorbent prepared by the method of example 1 above;
test No. 2 is a chitosan-manganese dioxide composite adsorbent prepared by the method of the above example 2;
test No. 3 shows a chitosan-manganese dioxide composite adsorbent produced by the method of example 3.
Table 1: bacteria removing effect
FIG. 4 shows the concentration of 0.5. + -. 0.1mg/m3And the environmental temperature is 25 +/-2 ℃, the environmental relative humidity is 50 +/-5%, and in a 100L sealed environmental chamber, the formaldehyde purifying effects of the common chitosan adsorbing material and the chitosan-manganese dioxide composite adsorbing material obtained by the preparation method of the embodiment 4 are shown in a contrast graph, so that the formaldehyde purifying effect of the chitosan-manganese dioxide composite adsorbing material is better. FIG. 4 shows chitosan/MnO for chitosan-manganese dioxide composite adsorbent2"means.
FIG. 5 shows the formaldehyde purification of the conventional chitosan adsorbent and the chitosan-manganese dioxide composite adsorbent obtained by the preparation method of the above example 4 at different filtration rates in the air duct systemResistance versus schematic. As can be seen from FIG. 5, the chitosan-manganese dioxide composite adsorbing material is arranged in the air duct systemIs relatively less resistive. FIG. 5 shows "Chitosan/MnO" for chitosan-manganese dioxide composite adsorbent2"means.
The working principle of the invention is as follows:
theoretically, an addition-dehydration reaction can occur between formaldehyde and chitosan, and the reaction principle is as shown in fig. 3 below. In the process of removing formaldehyde, manganese dioxide plays a role in catalytic oxidation. Its surface active group O2 -And the OH free radical portion is oxidized to form carbon dioxide and possibly water, but the formed water may continue to dissociate into 0H free radicals to participate in the reaction of oxidizing formaldehyde.
FIG. 3 the principle of purifying formaldehyde by chitosan
The antibacterial mechanism of chitosan mainly comprises ① surface action, interaction of protonated amino of chitosan and negative charges on the surface of microbial cell membrane to influence the structure of cell wall and cell membrane and change the permeability of cell to cause bacterial death, ② surface film forming, easy adsorption of macromolecular chitosan on the surface of bacteria to form macromolecular film to change the selective permeability of cell membrane and prevent normal transportation of nutrient substance to achieve the effects of sterilization and bacteriostasis, ③ entering thallus, easy entry of small molecular weight chitosan into cell and combination with negatively charged substance (nucleic acid protein) to interfere normal metabolism of thallus to destroy the physiological function.
The above-mentioned embodiments are only for illustrating the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and to carry out the same, and the present invention shall not be limited to the embodiments, i.e. the equivalent changes or modifications made within the spirit of the present invention shall fall within the scope of the present invention.
Claims (8)
1. A preparation method of a chitosan-manganese dioxide composite adsorption material is characterized by comprising the following steps:
step 1, preparing a redox reaction base solution: fully dissolving potassium permanganate powder in distilled water, adding oleic acid into the solution, and stirring to form O/W emulsion;
step 2, soaking: soaking chitosan degraded fiber as a base material in an oxidation-reduction reaction base solution, and standing for 24 hours at room temperature;
step 3; cleaning: washing the soaked chitosan degradable fiber with absolute ethyl alcohol to remove unreacted oleic acid, and washing with distilled water to remove residual ethyl alcohol;
and 4, drying the cleaned chitosan degradation fiber at 70 ℃ for 6 hours.
2. The preparation method of the chitosan-manganese dioxide composite adsorbing material as claimed in claim 1, wherein in the step 1, the specific method for preparing the redox reaction base solution is as follows: at room temperature, dispersing potassium permanganate powder in distilled water, and stirring for 20-30 minutes at a stirring speed of 800 revolutions per minute by using a magnetic stirrer to completely dissolve potassium permanganate; and dropwise adding oleic acid into the solution, and stirring for 4-6 minutes at the stirring speed of 800 revolutions per minute by adopting a magnetic stirrer to form O/W emulsion.
3. The preparation method of the chitosan-manganese dioxide composite adsorbing material as claimed in claim 1, wherein the raw materials for preparing the redox reaction base solution are as follows in parts by weight: 500 parts of distilled water, 0.5-1 part of potassium permanganate and 4.45-8.9 parts of oleic acid.
4. The preparation method of the chitosan-manganese dioxide composite adsorbing material as claimed in claim 3, wherein the raw materials for preparing the redox reaction base solution are as follows in parts by weight: 500 parts of distilled water, 0.5 part of potassium permanganate and 8.9 parts of oleic acid.
5. The preparation method of the chitosan-manganese dioxide composite adsorbing material as claimed in claim 1, wherein the mass ratio of the chitosan degradation fiber to the redox reaction base solution is 1: 100 to 130.
6. The preparation method of the chitosan-manganese dioxide composite adsorbing material as claimed in claim 1, wherein an emulsion obtained by mixing potassium permanganate and oleic acid is subjected to an oxidation-reduction reaction, and manganese dioxide generated by the reaction is in-situ deposited on the surface of the chitosan degraded fiber.
7. The method for preparing the chitosan-manganese dioxide composite adsorbing material according to claim 1, wherein the chitosan degrading fiber is made of chitosan needle punched cloth.
8. A chitosan-manganese dioxide composite adsorbing material prepared by the method for preparing a chitosan-manganese dioxide composite adsorbing material according to any one of claims 1 to 7.
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