CN114934385A - Cellulose acetate based composite aerogel and preparation method and application thereof - Google Patents
Cellulose acetate based composite aerogel and preparation method and application thereof Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- D06M15/61—Polyamines polyimines
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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
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
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- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
- D06M2101/08—Esters or ethers of cellulose
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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
Abstract
The invention discloses a cellulose acetate based composite aerogel and a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing cellulose acetate nanofibers with an oxidant aqueous solution to obtain a mixed solution; (2) adding a surface modification substance into the mixed solution, and reacting at 0-90 ℃ to obtain a cellulose acetate based composite material; (3) freeze-drying the cellulose acetate based composite material to obtain cellulose acetate based composite aerogel; wherein, the surface modification substance is selected from one or more of aromatic amine, pyrrole and poly 3, 4-vinyl dioxythiophene; the ratio of the volume of the surface-modifying substance to the mass of the cellulose acetate nanofibers is (5 to 25) μ L (0.5 to 2) g. The preparation method can obtain the cellulose acetate based composite aerogel with higher adsorption efficiency and adsorption capacity to Cr (VI) ions.
Description
Technical Field
The invention relates to a composite aerogel and a preparation method and application thereof, in particular to a cellulose acetate based composite aerogel and a preparation method and application thereof.
Background
Heavy metal contamination refers to environmental contamination caused by heavy metals or compounds thereof. Heavy metal pollution is mainly manifested in water pollution. Chromium is a common and hazardous pollutant in heavy metal water pollution. The main existing forms of chromium in nature are Cr (VI) and Cr (III), wherein the Cr (VI) can bring lasting harm to human health and ecological environment due to the characteristics of contact sensitization, inhalation carcinogenesis, possible genetic gene defect and high mobility.
At present, the treatment methods for cr (vi) in water mainly include chemical precipitation, adsorption, electrochemical methods, membrane separation, and the like. The traditional Cr (VI) treatment methods have the disadvantages of high cost, low efficiency, poor treatment effect, easy secondary pollution and the like in different degrees. The in-situ reduction adsorption method is a relatively efficient and environment-friendly treatment means. In the in-situ reduction adsorption method, the aerogel material becomes a novel adsorption material due to the advantages of low density, high porosity, high specific surface area and the like. However, the existing aerogel materials have the defects of high production cost, complex preparation process, poor adsorption capacity, easy secondary pollution and the like. Therefore, it is highly desirable to develop an aerogel material that is inexpensive to produce and has good adsorption properties.
Disclosure of Invention
In view of the above, a first object of the present invention is to provide a method for preparing a cellulose acetate based composite aerogel, which is simple to operate and low in preparation cost, and the obtained cellulose acetate based composite aerogel has high cr (vi) adsorption efficiency and adsorption capacity.
The second purpose of the invention is to provide a cellulose acetate based composite aerogel, which has higher adsorption efficiency and adsorption capacity to Cr (VI).
The third purpose of the invention is to provide the application of the cellulose acetate based composite aerogel in sewage treatment.
The invention adopts the following technical scheme to achieve the purpose.
In one aspect, the invention provides a preparation method of cellulose acetate based composite aerogel, which comprises the following steps:
(1) mixing cellulose acetate nanofibers with an oxidant aqueous solution to obtain a mixed solution;
(2) adding a surface modification substance into the mixed solution, and reacting at 0-90 ℃ to obtain a cellulose acetate base composite material;
(3) freeze-drying the cellulose acetate based composite material to obtain cellulose acetate based composite aerogel;
wherein the surface modification substance is selected from one or more of aromatic amine, pyrrole and poly 3, 4-vinyl dioxythiophene;
wherein the ratio of the volume of the surface-modifying substance to the mass of the cellulose acetate nanofibers is (5-25) μ L (0.5-2) g.
In the step (2), the reaction temperature may be 0 to 90 ℃, and preferably 5 to 80 ℃. The reaction time can be 2-8 h, preferably 4-6 h. Therefore, the cost can be saved, and the good adsorption performance of the cellulose acetate base composite aerogel is ensured.
In the step (2), the addition amount of the surface modification substance needs to be controlled, so that the ratio of the volume of the surface modification substance to the mass of the cellulose acetate nanofiber is (5-25) microliter (0.5-2) g; preferably (10-20) μ L (0.8-1.5) g. Therefore, the adsorption capacity of the cellulose acetate based composite aerogel on Cr (VI) can be effectively improved.
According to some preferred embodiments of the present invention, the ratio of the volume of the surface modification substance to the mass of the cellulose acetate nanofibers is (15-20) μ L, (1.1-1.3) g, such that the adsorption capacity of the prepared cellulose acetate based composite aerogel on cr (vi) can reach 40-58 mg/g.
The cellulose acetate-based composite aerogel is prepared by taking the cellulose acetate nanofibers as the raw materials, and has the advantages of simple operation, mild experimental conditions, cheap and easily-obtained raw materials and low production cost.
In addition, the cellulose acetate based composite aerogel prepared by the preparation method has higher adsorption capacity and adsorption efficiency on Cr (VI), and does not cause secondary pollution to the environment. According to some embodiments of the invention, the adsorption capacity of the cellulose acetate based composite aerogel of the invention on Cr (VI) ions can reach 30-58 mg/g, and preferably 40-58 mg/g. The adsorption process can reach the adsorption balance in 1.5-4 h, preferably 1.5-3 h, and more preferably 1.5-2 h.
In the invention, the cellulose acetate nanofiber can adopt conventional cellulose acetate nanofibers, preferably cellulose acetate nanofibers with the diameter of 100-1000 nm and the length of 20-2000 nm, and more preferably the cellulose acetate nanofibers prepared by the method. The oxidant can be one or more selected from ammonium persulfate, ferric trichloride and hydrogen peroxide, and is preferably ammonium persulfate or ferric trichloride. The surface modifying substance may be selected from one or more of aromatic amines, pyrrole and poly 3, 4-ethylenedioxythiophene, preferably aniline, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, toluidine, 2-naphthylamine, pyrrole or poly 3, 4-ethylenedioxythiophene, more preferably aniline or pyrrole. This helps to obtain cellulose acetate based composite aerogel having good adsorption property to cr (vi) ions.
According to the preparation method of the invention, preferably, the cellulose acetate nanofiber has a diameter of 100-1000 nm and a length of 20-2000 nm.
According to some embodiments of the invention, the cellulose acetate nanofibers have a diameter of 100 to 500nm and a length of 100 to 800 nm. This further contributes to obtaining a loose and porous cellulose acetate based composite aerogel.
According to the preparation method of the present invention, preferably, the mass concentration of the cellulose acetate nanofibers in the mixed solution is 5 to 30 wt%.
According to some embodiments of the present invention, the mixed solution contains cellulose acetate nanofibers in a mass concentration of 10 to 15 wt%.
According to the preparation method of the invention, preferably, the oxidant is selected from one or more of ammonium persulfate, ferric trichloride and hydrogen peroxide.
According to the preparation method of the invention, preferably, the mass concentration of the oxidant in the oxidant aqueous solution is 1-10 wt%.
According to some preferred embodiments of the invention, the oxidizing agent is selected from ammonium persulfate or ferric trichloride. In the oxidant aqueous solution, the mass concentration of the oxidant is 2-5 wt%.
In step (3) of the present invention, the temperature of freeze-drying may be-30 to-80 deg.C, preferably-40 to-70 deg.C. The freeze drying time can be 24-72 hours, preferably 36-48 hours. Therefore, not only can energy be saved, but also loose and porous cellulose acetate base composite aerogel can be obtained.
According to the preparation method of the present invention, preferably, the temperature of freeze-drying is-40 to-70 ℃.
According to the preparation method of the present invention, preferably, the cellulose acetate nanofibers are prepared by a method comprising the steps of:
1) dissolving cellulose acetate in a solvent to obtain a spinning solution;
2) carrying out electrostatic spinning on the spinning solution, crushing and drying to obtain the cellulose acetate nanofiber;
wherein the mass concentration of the cellulose acetate in the spinning solution is 5-45 wt%.
According to the preparation method of the present invention, preferably, in step 1), the solvent is selected from one or more of acetone, N dimethylformamide, N dimethylacetamide, dichloromethane, tetrahydrofuran, and dimethylsulfoxide. In certain embodiments, the solvent is a mixed solvent of acetone and N, N dimethylformamide; wherein the volume ratio of the acetone to the N, N-dimethylformamide is 1.8-3.5: 1, preferably 2-3: 1. In other embodiments, the solvent is a mixed solvent of acetone and N, N dimethylacetamide; wherein the volume ratio of the acetone to the N, N-dimethylacetamide is 1.8-3.5: 1, preferably 2-3: 1.
According to some preferred embodiments of the present invention, the cellulose acetate nanofibers are prepared by a process comprising:
1) dissolving cellulose acetate in a mixed solvent of acetone and N, N-dimethylformamide to obtain a spinning solution;
2) carrying out electrostatic spinning on the spinning solution, crushing and drying to obtain the cellulose acetate nanofiber;
wherein the mass concentration of the cellulose acetate in the spinning solution is 15-20 wt%. The cellulose acetate nano-fiber prepared in the way can better react with a surface modification substance to obtain the cellulose acetate based composite aerogel with good adsorption performance.
In the invention, the technological parameters of electrostatic spinning can be set as follows: the spinning distance between the spinning nozzle (such as a #21 flat-mouth needle) and the receiving device is 10-20 cm, for example 15 cm; the positive voltage of the spinning voltage is 12-25 kV, such as 18 kV; the negative pressure is 0 to-8 kV, such as-2 kV; the propelling speed is 0.010-0.020 mL/min, such as 0.015 mL/min; the ambient humidity is set to 20-40%, for example 30%.
In another aspect, the invention provides a cellulose acetate based composite aerogel prepared by the preparation method.
In yet another aspect, the present invention provides use of a cellulose acetate based composite aerogel in sewage treatment. In particular to application of cellulose acetate based composite aerogel in treating sewage containing Cr (VI) ions. According to some embodiments of the invention, the cellulose acetate based composite aerogel is placed in sewage containing Cr (VI) ions for adsorption, wherein the pH value of the sewage is 2-6. The adsorption time can be 1-4 h; preferably 1.5 to 3 hours.
The cellulose acetate-based composite aerogel is prepared by taking the cellulose acetate nanofibers as the raw materials, and has the advantages of simple operation, mild experimental conditions, cheap and easily obtained raw materials and low production cost. In addition, the cellulose acetate based composite aerogel prepared by the preparation method has higher adsorption capacity and adsorption efficiency on Cr (VI) ions, and does not cause secondary pollution to the environment.
Drawings
FIG. 1 is a scanning electron micrograph of cellulose acetate nanofibers.
Fig. 2 is a scanning electron micrograph of the cellulose acetate-based composite material.
Fig. 3 is a real object diagram of the cellulose acetate-based composite aerogel according to example 1.
Fig. 4 is a graph of adsorption capacity of the cellulose acetate based composite aerogel of example 1.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
The test method is described below:
(1) and (3) testing the adsorption capacity: taking 40mg of cellulose acetate based composite aerogel, putting the cellulose acetate based composite aerogel into 40ml of simulated wastewater containing Cr (VI) ions, wherein the pH value of the simulated wastewater is 2, and the initial concentration of the Cr (VI) ions in the simulated wastewater is c 0 (in mg/l); adsorption was carried out for 4h, and the Cr (VI) ion concentration c (in mg/l) in the simulated wastewater was measured. The adsorption capacity was calculated according to the following formula:
adsorption capacity (mg/g) ═ c 0 -c)(mg/g)
Wherein, the concentration of Cr (VI) ions is tested by an ultraviolet spectrophotometry.
Examples 1 to 3 and comparative examples 1 to 3
(1) According to the formula shown in the table 1, cellulose acetate is dissolved in a solvent, and the solution is stirred for 6 hours at room temperature to obtain a uniform spinning solution;
(2) carrying out electrostatic spinning on the spinning solution to obtain cellulose acetate nano long fibers; placing the cellulose acetate nano long fibers in a wall breaking machine to be broken and then drying to obtain cellulose acetate nano fibers;
the specific parameters of electrostatic spinning are as follows: the spinning distance is 15cm, the positive pressure is 18kV, the negative pressure is-2 kV, the propelling speed is 0.015mL/min, and the environmental humidity is 30%;
(3) placing cellulose acetate nanofibers in a mold with the inner diameter of 3cm, adding an oxidant aqueous solution, and uniformly mixing to obtain a mixed solution;
(4) adding a surface modification substance into the mixed solution, and carrying out polymerization reaction for 6 hours to obtain a cellulose acetate based composite material;
(5) and (3) putting the cellulose acetate based composite material into a freeze dryer for freeze-drying for 48 hours to obtain the cellulose acetate based composite aerogel.
The adsorption capacity of the cellulose acetate based composite aerogel in simulated wastewater with Cr (VI) ion concentrations of 0.1mg/l, 0.15mg/l and 0.2mg/l was respectively tested, and the results are shown in Table 2.
Fig. 1 is a scanning electron micrograph of the cellulose acetate nanofibers of example 1. Fig. 2 is a scanning electron micrograph of the cellulose acetate-based composite material of example 1. As can be seen from FIGS. 1-2, the modified fiber surface has attachments. Fig. 3 is a physical diagram of the cellulose acetate-based composite aerogel according to example 1, and it can be seen that the cellulose acetate-based composite aerogel according to the present invention has a loose porous structure. Fig. 4 is an adsorption curve diagram of the cellulose acetate-based composite aerogel of example 1, and it can be seen that adsorption equilibrium is substantially reached after 2 hours of adsorption, and the adsorption efficiency is high. And the cellulose acetate based composite aerogel shows higher adsorption capacity in simulated wastewater with Cr (VI) ion concentrations of 0.1mg/l, 0.15mg/l and 0.2 mg/l.
TABLE 1
TABLE 2
As can be seen from table 2, the cellulose acetate based composite aerogel according to the present invention has a higher adsorption capacity for cr (vi) ions.
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (10)
1. The preparation method of the cellulose acetate based composite aerogel is characterized by comprising the following steps of:
(1) mixing cellulose acetate nanofibers with an oxidant aqueous solution to obtain a mixed solution;
(2) adding a surface modification substance into the mixed solution, and reacting at 0-90 ℃ to obtain a cellulose acetate based composite material;
(3) freeze-drying the cellulose acetate based composite material to obtain cellulose acetate based composite aerogel;
wherein the surface modification substance is selected from one or more of aromatic amine, pyrrole and poly 3, 4-vinyl dioxythiophene;
wherein the ratio of the volume of the surface-modifying substance to the mass of the cellulose acetate nanofibers is (5-25) μ L (0.5-2) g.
2. The method according to claim 1, wherein the cellulose acetate nanofibers have a diameter of 100 to 1000nm and a length of 20 to 2000 nm.
3. The method according to claim 1, wherein the mixed solution contains cellulose acetate nanofibers at a mass concentration of 5 to 30 wt%.
4. The preparation method according to claim 1, wherein the oxidant is one or more selected from ammonium persulfate, ferric trichloride and hydrogen peroxide.
5. The method according to claim 1, wherein the aqueous solution of the oxidizing agent has a mass concentration of the oxidizing agent of 1 to 10 wt%.
6. The method according to claim 1, wherein the temperature of the freeze-drying is-40 to-70 ℃.
7. The preparation method according to claim 1, wherein the cellulose acetate nanofibers are prepared by a process comprising:
1) dissolving cellulose acetate in a solvent to obtain a spinning solution;
2) carrying out electrostatic spinning on the spinning solution, crushing and drying to obtain the cellulose acetate nanofiber;
wherein the mass concentration of the cellulose acetate in the spinning solution is 5-45 wt%.
8. The method according to claim 7, wherein the solvent is selected from one or more of acetone, N-dimethylformamide, N-dimethylacetamide, dichloromethane, tetrahydrofuran, and dimethylsulfoxide in step 1).
9. A cellulose acetate-based composite aerogel, characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. Use of the cellulose acetate based composite aerogel according to claim 9 in sewage treatment.
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