CN114618403A - Preparation method of ferrocene hybridized chitosan-based aerogel, product and application of product - Google Patents
Preparation method of ferrocene hybridized chitosan-based aerogel, product and application of product Download PDFInfo
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- CN114618403A CN114618403A CN202210203332.4A CN202210203332A CN114618403A CN 114618403 A CN114618403 A CN 114618403A CN 202210203332 A CN202210203332 A CN 202210203332A CN 114618403 A CN114618403 A CN 114618403A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a preparation method of ferrocene hybridized chitosan-based aerogel, a product and application thereof, wherein the preparation method comprises the steps of dissolving chitosan in an acetic acid aqueous solution, mixing the chitosan with an alcohol solution of ferrocene formaldehyde, and reacting for 1-5 hours at 20-80 ℃ to obtain hydrogel; and directly soaking the hydrogel in alkali liquor for 3-12 hours, taking out the hydrogel, and freeze-drying the hydrogel to obtain the ferrocene hybridized chitosan-based aerogel. The preparation method of the ferrocene hybridized chitosan-based aerogel does not need chemical crosslinking, and can be prepared only by soaking in alkali liquor and then freeze-drying; the ferrocene hybridized chitosan-based aerogel prepared by the invention not only has excellent phosphate adsorption performance, but also can rapidly degrade organic dye, and the degradation rate within 1 hour can reach 95%.
Description
Technical Field
The invention belongs to the technical field of aerogel preparation, and particularly relates to a preparation method of ferrocene hybridized chitosan-based aerogel, a product and application thereof.
Background
The aerogel has a very large specific surface area, an easily-modified surface and a unique porous structure, so that the aerogel becomes an ideal adsorbent for treating wastewater, and can meet the adsorption requirements on oils, dyes and heavy metal ions.
The chitosan aerogel is a biomass aerogel material prepared by chemical crosslinking or physical crosslinking, has the characteristics of large specific surface area and high porosity of a porous aerogel material, and is an environment-friendly oil absorption material with great development potential after surface hydrophobization treatment.
However, conventional chitosan aerogels tend to have poor phosphate adsorption properties and do not have the ability to degrade dyes.
Therefore, there is a need in the art for a novel chitosan-based aerogel having excellent adsorption properties to phosphate while being capable of degrading organic dyes.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of ferrocene hybridized chitosan-based aerogel.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of ferrocene hybridized chitosan-based aerogel comprises the following steps,
dissolving chitosan in an acetic acid aqueous solution, mixing the chitosan with an alcohol solution of ferrocenecarboxaldehyde, and reacting at the temperature of 20-80 ℃ for 1-5 hours to obtain hydrogel;
and directly soaking the hydrogel in alkali liquor for 3-12 hours, taking out, and freeze-drying to obtain the ferrocene hybridized chitosan-based aerogel.
As a preferred scheme of the preparation method of the ferrocene hybridized chitosan-based aerogel, the preparation method comprises the following steps: the mass ratio of the chitosan to the ferrocene formaldehyde is 1: 0.5-1: 4.
As a preferred scheme of the preparation method of the ferrocene hybridized chitosan-based aerogel, the preparation method comprises the following steps: the mass ratio of the chitosan to the ferrocene formaldehyde is 1: 2.
As a preferred scheme of the preparation method of the ferrocene hybridized chitosan-based aerogel, the preparation method comprises the following steps: the alkali liquor is one or two of sodium hydroxide solution and sodium borohydride solution.
As a preferred scheme of the preparation method of the ferrocene hybridized chitosan-based aerogel, the preparation method comprises the following steps: the weight average molecular weight of the chitosan is 30000-500000.
As a preferred scheme of the preparation method of the ferrocene hybridized chitosan-based aerogel, the preparation method comprises the following steps: the concentration of the acetic acid aqueous solution is 1 wt%.
The invention further aims to overcome the defects in the prior art and provide application of a product prepared by the preparation method of the ferrocene hybridized chitosan-based aerogel in adsorbing organic dye molecules in water and degrading dyes in the presence of hydrogen peroxide, wherein the pH of the degrading dyes is 4-7, and the content of the hydrogen peroxide in the degrading dyes is 0.3-5 wt%.
Another objective of the present invention is to overcome the deficiencies in the prior art, and provide an application of ferrocene hybridized chitosan-based aerogel product in adsorbing phosphate in water, wherein the maximum adsorption amount of the aerogel on phosphate can reach 1596 mg/g.
The invention has the beneficial effects that:
the preparation method of the ferrocene hybridized chitosan-based aerogel does not need chemical crosslinking, and can be prepared only by soaking in alkali liquor and then freeze-drying; the ferrocene hybridized chitosan-based aerogel prepared by the invention not only has excellent phosphate adsorption performance, but also can rapidly degrade organic dye, and the degradation rate within 1 hour can reach 95%.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a photograph of ferrocene-hybridized chitosan-based aerogel prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope of the ferrocene-hybridized chitosan-based aerogel prepared in example 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Dissolving 1 g of chitosan with the weight-average molecular weight of 100000 in 1 wt% acetic acid aqueous solution, then mixing with a methanol solution (with the concentration of 0.25 g/ml) containing 2 g of ferrocene formaldehyde, and reacting at 50 ℃ for 5 hours to obtain hydrogel;
then, directly immersing the hydrogel into a sodium hydroxide-sodium borohydride mixed alkali solution (mass ratio is 1:1, concentration is 5 wt%) for soaking for 6 hours, taking out the hydrogel, and freeze-drying the hydrogel to obtain the ferrocene hybrid chitosan aerogel, wherein a photo of the prepared ferrocene hybrid chitosan aerogel is shown in figure 1.
Example 2
Dissolving 1 g of chitosan with the weight-average molecular weight of 50000 in 1 wt% acetic acid aqueous solution, then mixing with an ethanol solution (with the concentration of 0.25 g/ml) containing 1 g of ferrocene formaldehyde, and reacting at 80 ℃ for 2 hours to obtain hydrogel;
and then directly soaking the hydrogel into a sodium hydroxide solution (with the concentration of 5 wt%) for 12 hours, taking out, and freeze-drying to obtain the ferrocene hybrid chitosan aerogel.
Example 3
Dissolving 1 g of chitosan with the weight-average molecular weight of 300000 in a 1 wt% acetic acid aqueous solution, then mixing with a methanol solution (concentration of 0.25 g/ml) containing 3 g of ferrocenecarboxaldehyde, and reacting at 30 ℃ for 5 hours to obtain hydrogel;
and then directly immersing the hydrogel into a sodium borohydride solution (with the concentration of 5 wt%) for 10 hours, taking out, and freeze-drying to obtain the ferrocene hybrid chitosan aerogel.
Example 4
Dissolving 1 g of chitosan with the weight-average molecular weight of 500000 in a 1 wt% acetic acid aqueous solution, then mixing with an ethanol solution (with the concentration of 0.25 g/ml) containing 4 g of ferrocene carboxaldehyde, and reacting at 60 ℃ for 4 hours to obtain hydrogel;
and then directly immersing the hydrogel into a sodium hydroxide-sodium borohydride mixed alkali solution (the mass ratio is 1:1, and the concentration is 5 wt%) for soaking for 8 hours, taking out, and freeze-drying to obtain the ferrocene hybrid chitosan aerogel.
Example 5
(1) Structural characterization of the ferrocene hybrid chitosan aerogel:
the ferrocene hybrid chitosan aerogel prepared in example 1 was structurally characterized by scanning electron microscopy and BET technique and compared with chitosan aerogel not hybridized with ferrocene. The results are shown in FIG. 2 and Table 1.
(2) The adsorption performance of the ferrocene hybrid chitosan aerogel on phosphate is as follows:
0.05 g of the ferrocene hybrid chitosan aerogel prepared in the example 1-4 was weighed into 50 ml of potassium dihydrogen phosphate aqueous solution (pH 5) with the concentration of 250 mg/L, and stirred at 30 ℃ for 1 hour. And then taking the solution, filtering, and measuring the content of phosphorus by plasma inductance coupling plasma mass spectrometry so as to calculate the amount of phosphate adsorbed by the aerogel. The control was chitosan aerogel not hybridized with ferrocene. The results are shown in Table 2.
(3) Degradation performance of ferrocene hybrid chitosan aerogel on methylene blue dye:
weighing 0.03 g of the ferrocene hybrid chitosan aerogel prepared in the embodiment 1-4, putting the ferrocene hybrid chitosan aerogel into 50 ml of methylene blue aqueous solution with the concentration of 50 mg/L, adding 0.3-5 wt% of hydrogen peroxide, adjusting the pH value to be 4-7, and stirring for 1 hour at the temperature of 30 ℃. The control sample is chitosan aerogel without ferrocene hybridization.
The methylene blue content of the solution was detected spectrophotometrically.
The results are shown in Table 3.
TABLE 1
| Aperture (nanometer) | Hole area (square meter/gram) | Pore volume (cubic centimeter/gram) | |
| Comparative example | 11.49 | 21.71 | 0.062 |
| Example 1 | 6.32 | 5.00 | 0.0079 |
TABLE 2
TABLE 3
As can be seen from FIG. 2, the structure of the ferrocene hybridized chitosan aerogel is looser, and the chitosan aerogel presents more layered structures rather than porous structures.
The BET results listed in table 1 reveal a large reduction in pore size, pore area and pore volume, especially pore volume and pore area, relative to that before ferrocene hybridization. Theoretically, the adsorption sites of the ferrocene hybridized chitosan aerogel can be reduced, and the ion adsorption is not promoted.
However, the results in table 2 show that the ferrocene hybridization treated chitosan aerogel exhibited very high saturated adsorption amount to phosphate relative to the control example. In particular, in example 1, the saturated adsorption amount of phosphate was 20 times or more as large as that in the comparative example. More importantly, the saturated adsorption capacity of the ferrocene hybrid chitosan aerogel prepared by the invention to phosphate is far higher than the reported value of the existing literature.
As can be seen from table 3, the ferrocene hybrid chitosan aerogel prepared in examples 1 to 4 of the present invention has a high degradation capability to methylene blue in the presence of hydrogen peroxide, and the degradation rate in 1 hour can reach more than 92%, especially the degradation rate in 1 hour can reach more than 95%. Under the same conditions, the degradation rate of the control example to methylene blue is only 13%.
From the results, although the structure of the chitosan aerogel becomes more loose and the pore volume and the pore area are greatly shrunk after ferrocene hybridization modification, the adsorption of phosphate and the degradation of methylene blue are greatly improved.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of ferrocene hybridized chitosan-based aerogel is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
dissolving chitosan in an acetic acid aqueous solution, mixing the chitosan with an alcoholic solution of ferrocenecarboxaldehyde, and reacting at the temperature of 20-80 ℃ for 1-5 hours to obtain hydrogel;
and directly soaking the hydrogel in alkali liquor for 3-12 hours, taking out, and freeze-drying to obtain the ferrocene hybridized chitosan-based aerogel.
2. The preparation method of the ferrocene hybridized chitosan-based aerogel as in claim 1, wherein the preparation method comprises the following steps: the mass ratio of the chitosan to the ferrocene formaldehyde is 1: 0.5-1: 4.
3. A method for preparing ferrocene hybridized chitosan-based aerogel as claimed in claim 1 or 2, wherein: the mass ratio of the chitosan to the ferrocene formaldehyde is 1: 2.
4. A method for preparing ferrocene hybridized chitosan-based aerogel as claimed in claim 1 or 2, wherein: the alkali liquor is one or two of sodium hydroxide solution and sodium borohydride solution.
5. The preparation method of the ferrocene hybridized chitosan-based aerogel as in claim 1, wherein the preparation method comprises the following steps: the weight average molecular weight of the chitosan is 30000-500000.
6. The preparation method of the ferrocene hybridized chitosan-based aerogel as in claim 1, wherein the preparation method comprises the following steps: the concentration of the acetic acid aqueous solution is 1 wt%.
7. A product prepared by the preparation method of the ferrocene hybridized chitosan-based aerogel as in any one of claims 1 to 6.
8. Use of the product of claim 7 for adsorbing organic dye molecules in water and for degrading dyes in the presence of hydrogen peroxide.
9. The use of claim 8, wherein: the pH value of the degradation dye is 4-7, and the content of hydrogen peroxide in the degradation dye is 0.3-5 wt%.
10. Use of the product of claim 7 for adsorbing phosphate in water, wherein: the maximum adsorption capacity of the aerogel on phosphate can reach 1596 mg/g.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050107253A1 (en) * | 2001-12-21 | 2005-05-19 | Hiroyuki Sano | Adsorbent for phosphoric acid |
| US20070272902A1 (en) * | 2006-05-25 | 2007-11-29 | Aspen Aerogels, Inc. | Aerogel compositions with enhanced performance |
| CN103424449A (en) * | 2013-07-30 | 2013-12-04 | 浙江理工大学 | Ferrocene grafted chitosan-carbon nanotube-enzyme composite membrane modified three-dimensional graphene composite material and preparation method thereof |
| CN108421534A (en) * | 2018-02-08 | 2018-08-21 | 中山大学 | A kind of chitosan gel rubber material and preparation method thereof, wastewater treatment method and application |
| CN111393707A (en) * | 2020-04-08 | 2020-07-10 | 江西理工大学 | Preparation method of chitosan hybrid aerogel |
| CN113185749A (en) * | 2021-04-22 | 2021-07-30 | 长沙理工大学 | Preparation method of high-adsorbability chitosan aerogel |
| CN113754032A (en) * | 2021-08-25 | 2021-12-07 | 同济大学 | Ferrocene modified polyaniline/carbon nanotube composite electrode capable of selectively removing phosphate ions and preparation method and application thereof |
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- 2022-03-03 CN CN202210203332.4A patent/CN114618403B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050107253A1 (en) * | 2001-12-21 | 2005-05-19 | Hiroyuki Sano | Adsorbent for phosphoric acid |
| US20070272902A1 (en) * | 2006-05-25 | 2007-11-29 | Aspen Aerogels, Inc. | Aerogel compositions with enhanced performance |
| CN103424449A (en) * | 2013-07-30 | 2013-12-04 | 浙江理工大学 | Ferrocene grafted chitosan-carbon nanotube-enzyme composite membrane modified three-dimensional graphene composite material and preparation method thereof |
| CN108421534A (en) * | 2018-02-08 | 2018-08-21 | 中山大学 | A kind of chitosan gel rubber material and preparation method thereof, wastewater treatment method and application |
| CN111393707A (en) * | 2020-04-08 | 2020-07-10 | 江西理工大学 | Preparation method of chitosan hybrid aerogel |
| CN113185749A (en) * | 2021-04-22 | 2021-07-30 | 长沙理工大学 | Preparation method of high-adsorbability chitosan aerogel |
| CN113754032A (en) * | 2021-08-25 | 2021-12-07 | 同济大学 | Ferrocene modified polyaniline/carbon nanotube composite electrode capable of selectively removing phosphate ions and preparation method and application thereof |
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