CN114934385B - 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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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- 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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- C—CHEMISTRY; METALLURGY
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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
- C08J2201/048—Elimination of a frozen liquid phase
- 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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- C—CHEMISTRY; METALLURGY
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/16—Esters of inorganic acids
- C08J2301/18—Cellulose nitrate
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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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- 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
- 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 nanofiber with an oxidant aqueous solution to obtain a mixed solution; (2) Adding a surface modifying 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 modifying 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 nanofiber is (5-25) mu L (0.5-2) g. The preparation method of the invention 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 pollution caused by heavy metals or compounds thereof. Heavy metal pollution is mainly manifested in water pollution. Chromium is a common, hazardous and huge contaminant in heavy metal water pollution. The main existing forms of chromium in nature are Cr (VI) and Cr (III), wherein Cr (VI) can bring permanent harm to human health and ecological environment because of the characteristics of contact sensitization, inhalation carcinogenesis, possible genetic defects and high migration.
At present, the treatment method for Cr (VI) in the water body mainly comprises a chemical precipitation method, an adsorption method, an electrochemical method, a membrane separation method and the like. The traditional Cr (VI) treatment methods have the defects of over high cost, low efficiency, poor treatment effect, easiness in causing secondary pollution and the like at 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 material has the defects of high production cost, complex preparation process, poor adsorption capacity, easiness in causing secondary pollution and the like. Therefore, development of an aerogel material having low preparation cost and good adsorption performance is needed.
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 adsorption efficiency and adsorption capacity for Cr (VI).
The second object of the present invention is to provide a cellulose acetate based composite aerogel having higher adsorption efficiency and adsorption capacity for Cr (VI).
A third object of the present invention is to provide a use of a cellulose acetate based composite aerogel in sewage treatment.
The invention adopts the following technical scheme to realize the aim.
In one aspect, the invention provides a method for preparing cellulose acetate based composite aerogel, comprising the following steps:
(1) Mixing cellulose acetate nanofiber with an oxidant aqueous solution to obtain a mixed solution;
(2) Adding a surface modifying 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 modifying 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 nanofiber is (5-25) mu L (0.5-2) g.
In step (2) of the present invention, the reaction temperature may be 0 to 90℃and preferably 5 to 80 ℃. The reaction time may be 2 to 8 hours, preferably 4 to 6 hours. Therefore, the cost can be saved, and meanwhile, the good adsorption performance of the cellulose acetate based composite aerogel is ensured.
In the step (2) of the present invention, it is necessary to control the addition amount of the surface modifying substance so that the ratio of the volume of the surface modifying substance to the mass of the cellulose acetate nanofiber is (5 to 25) μl (0.5 to 2) g; preferably (10-20) mu L and (0.8-1.5) g. Thus, the adsorption capacity of the cellulose acetate based composite aerogel to Cr (VI) can be effectively improved.
According to some preferred embodiments of the present invention, the ratio of the volume of the surface modifying substance to the mass of the cellulose acetate nanofiber is (15-20) μl (1.1-1.3) g, and the adsorption capacity of the cellulose acetate based composite aerogel thus prepared on Cr (VI) can reach 40-58 mg/g.
The invention prepares the cellulose acetate based composite aerogel by taking the cellulose acetate nanofiber as the raw material, and has the advantages of simple operation, mild experimental conditions, low-cost 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 to Cr (VI), and cannot cause secondary pollution to the environment. According to some embodiments of the present invention, the adsorption capacity of the cellulose acetate based composite aerogel of the present invention to Cr (VI) ions may reach 30 to 58mg/g, preferably 40 to 58mg/g. The adsorption process may reach adsorption equilibrium at 1.5 to 4 hours, preferably 1.5 to 3 hours, more preferably 1.5 to 2 hours.
In the invention, the cellulose acetate nanofiber can be a conventional cellulose acetate nanofiber, preferably a cellulose acetate nanofiber with the diameter of 100-1000 nm and the length of 20-2000 nm, and more preferably a cellulose acetate nanofiber prepared by the invention. The oxidant can be selected from one or more of 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-vinyldioxythiophene, preferably aniline, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, toluidine, 2-naphthylamine, pyrrole or poly 3, 4-vinyldioxythiophene, more preferably aniline or pyrrole. Thus being beneficial to obtaining the cellulose acetate based composite aerogel with good adsorption performance on Cr (VI) ions.
According to the preparation method of the present invention, preferably, the cellulose acetate nanofiber has a diameter of 100 to 1000nm and a length of 20 to 2000nm.
According to some embodiments of the invention, the cellulose acetate nanofiber has a diameter of 100 to 500nm and a length of 100 to 800nm. This is more conducive to obtaining loose porous cellulose acetate based composite aerogels.
According to the preparation method of the present invention, preferably, the mass concentration of the cellulose acetate nanofiber in the mixed solution is 5 to 30wt%.
According to some embodiments of the invention, the mass concentration of the cellulose acetate nanofiber in the mixed solution is 10-15 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 production method of the present invention, preferably, the mass concentration of the oxidizing agent in the aqueous oxidizing agent solution is 1 to 10wt%.
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 ℃, preferably-40 to-70 ℃. The time for freeze-drying may be 24 to 72 hours, preferably 36 to 48 hours. Thus not only saving energy, but also obtaining loose and porous cellulose acetate base composite aerogel.
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 nanofiber is prepared by comprising the steps of:
1) Dissolving cellulose acetate in a solvent to obtain spinning solution;
2) Carrying out electrostatic spinning, crushing and drying on the spinning solution to obtain the cellulose acetate nanofiber;
wherein, in the spinning solution, the mass concentration of the cellulose acetate is 5 to 45 weight percent.
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, methylene chloride, 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, and is 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 nanofiber is prepared by:
1) Dissolving cellulose acetate in a mixed solvent of acetone and N, N-dimethylformamide to obtain spinning solution;
2) Carrying out electrostatic spinning, crushing and drying on the spinning solution to obtain the cellulose acetate nanofiber;
wherein, in the spinning solution, the mass concentration of the cellulose acetate is 15-20wt%. The cellulose acetate nanofiber prepared in this way can better react with the 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 spinneret (such as #21 flat needle) and the receiving device is 10-20 cm, such as 15cm; the positive pressure of the spinning voltage is 12-25 kV, such as 18kV; the negative voltage is 0 to-8 kV, such as-2 kV; the propelling speed is 0.010-0.020 mL/min, such as 0.015mL/min; the ambient humidity is set to 20-40%, for example 30%.
On the other hand, the invention provides the cellulose acetate-based composite aerogel prepared by the preparation method.
In yet another aspect, the present invention provides the use of a cellulose acetate based composite aerogel in the treatment of sewage. In particular to an 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 a wastewater containing Cr (VI) ions for adsorption, wherein the pH of the wastewater is 2-6. The adsorption time can be 1-4 h; preferably 1.5 to 3 hours.
The invention prepares the cellulose acetate based composite aerogel by taking the cellulose acetate nanofiber as the raw material, and has the advantages of simple operation, mild experimental conditions, low-cost 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 cannot cause secondary pollution to the environment.
Drawings
Fig. 1 is a scanning electron microscope photograph of cellulose acetate nanofibers.
Fig. 2 is a scanning electron micrograph of a cellulose acetate based composite.
FIG. 3 is a physical view of the cellulose acetate based composite aerogel of 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 specific examples, but the scope of the present invention is not limited thereto.
The test method is described as follows:
(1) Adsorption capacity test: 40mg of cellulose acetate based composite aerogel is taken,placing in 40ml of simulated wastewater containing Cr (VI) ions, wherein the pH 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); and (3) adsorbing for 4 hours, and testing the concentration c (unit is mg/l) of Cr (VI) ions in the simulated wastewater. 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 ultraviolet spectrophotometry.
Examples 1 to 3 and comparative examples 1 to 3
(1) According to the formula of Table 1, cellulose acetate is dissolved in a solvent and 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; breaking cellulose acetate nanometer long fibers in a wall breaking machine, and drying to obtain cellulose acetate nanometer fibers;
wherein, the specific parameters of the electrostatic spinning are set as follows: the spinning distance is 15cm, the positive pressure is 18kV, the negative pressure is-2 kV, the propulsion speed is 0.015mL/min, and the environmental humidity is 30%;
(3) Placing cellulose acetate nanofiber in a die with the inner diameter of 3cm, adding an oxidant aqueous solution, and uniformly mixing to obtain a mixed solution;
(4) Adding a surface modifying 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, and freeze-drying for 48 hours to obtain the cellulose acetate-based composite aerogel.
The adsorption capacities of the cellulose acetate based composite aerogel in the simulated wastewater having Cr (VI) ion concentrations of 0.1mg/l, 0.15mg/l and 0.2mg/l were respectively tested, and the results are shown in table 2.
Fig. 1 is a scanning electron micrograph of the cellulose acetate nanofiber of example 1. Fig. 2 is a scanning electron micrograph of the cellulose acetate based composite of example 1. As can be seen from fig. 1 to 2, the modified fiber surface has an attached matter. Fig. 3 is a physical diagram of the cellulose acetate based composite aerogel of example 1, and it can be seen that the cellulose acetate based composite aerogel of the present invention has a loose porous structure. Fig. 4 is an adsorption graph of the cellulose acetate based composite aerogel of example 1, and it can be seen that adsorption equilibrium is basically reached at the time of adsorption for 2 hours, and the adsorption efficiency is high. And the cellulose acetate based composite aerogel has higher adsorption capacity in the simulated wastewater with the concentration of Cr (VI) ions 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 of 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 modifications, improvements, substitutions, and the like, which may occur to those skilled in the art, fall within the scope of the present invention without departing from the spirit of the invention.
Claims (8)
1. A method for preparing cellulose acetate based composite aerogel for treating wastewater containing Cr (VI) ions, comprising the steps of:
(1) Mixing cellulose acetate nanofiber with an oxidant aqueous solution to obtain a mixed solution;
(2) Adding a surface modifying substance into the mixed solution, and reacting at 80-90 ℃ to obtain a cellulose acetate-based composite material;
(3) Freeze-drying the cellulose acetate-based composite material to obtain cellulose acetate-based composite aerogel for treating sewage containing Cr (VI) ions;
wherein the surface modifying substance is aniline; the diameter of the cellulose acetate nanofiber is 100-1000 nm, and the length is 20-2000 nm; in the oxidant aqueous solution, the mass concentration of the oxidant is 2-5wt%; in the mixed solution, the mass concentration of the cellulose acetate nanofiber is 5-30wt%;
wherein the ratio of the volume of the surface modifying substance to the mass of the cellulose acetate nanofiber is (10-20) mu L (0.8-1.3) g.
2. A method for preparing cellulose acetate based composite aerogel for treating wastewater containing Cr (VI) ions, comprising the steps of:
(1) Mixing cellulose acetate nanofiber with an oxidant aqueous solution to obtain a mixed solution;
(2) Adding a surface modifying substance into the mixed solution, and reacting at 0-5 ℃ to obtain a cellulose acetate-based composite material;
(3) Freeze-drying the cellulose acetate-based composite material to obtain cellulose acetate-based composite aerogel for treating sewage containing Cr (VI) ions;
wherein the surface modifying substance is pyrrole; the diameter of the cellulose acetate nanofiber is 100-1000 nm, and the length is 20-2000 nm; in the oxidant aqueous solution, the mass concentration of the oxidant is 2-5wt%; in the mixed solution, the mass concentration of the cellulose acetate nanofiber is 5-30wt%;
wherein the ratio of the volume of the surface modifying substance to the mass of the cellulose acetate nanofiber is (10-20) mu L (0.8-1.3) g.
3. The preparation method according to claim 1 or 2, wherein the oxidizing agent is one or more selected from ammonium persulfate, ferric trichloride and hydrogen peroxide.
4. The process according to claim 1 or 2, wherein the freeze-drying temperature is-40 to-70 ℃.
5. The method of preparing according to claim 1 or 2, wherein the cellulose acetate nanofiber is prepared by comprising the steps of:
1) Dissolving cellulose acetate in a solvent to obtain spinning solution;
2) Carrying out electrostatic spinning, crushing and drying on the spinning solution to obtain the cellulose acetate nanofiber;
wherein, in the spinning solution, the mass concentration of the cellulose acetate is 5 to 45 weight percent.
6. The method according to claim 5, wherein in step 1), the solvent is one or more selected from the group consisting of acetone, N-dimethylformamide, N-dimethylacetamide, methylene chloride, tetrahydrofuran, and dimethylsulfoxide.
7. A cellulose acetate based composite aerogel for treating sewage containing Cr (VI) ions, characterized by being prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the cellulose acetate based composite aerogel according to claim 7 for treating sewage containing Cr (VI) ions.
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| CN101851398A (en) * | 2010-05-12 | 2010-10-06 | 北京理工大学 | Conductive polymer aerogel and preparation method thereof |
| WO2014208917A2 (en) * | 2013-06-25 | 2014-12-31 | 동국대학교 산학협력단 | Holocellulose aerogel and heavy metal adsorbent using same |
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