CN111875006A - Preparation method of biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode - Google Patents
Preparation method of biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode Download PDFInfo
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Abstract
A preparation method of a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode, uses cheap natural biomass with natural plant fiber sponge structure such as agricultural processing wastes such as shaddock peel and bagasse as raw materials, prepares N, P co-doped carbon aerogel with developed mesoporous structure through the working procedures of pre-carbonization, high-temperature carbonization and the like, further compounds N, P co-doped carbon aerogel with chitosan to prepare an electro-adsorption membrane electrode, the prepared biomass source N, P co-doped carbon aerogel/chitosan composite membrane electrode has high specific surface area, good conductivity and chemical stability, when the uranium adsorbent is used for the uranium in the uranium-bearing wastewater of the electro-adsorption separation, the uranium adsorbent has high uranium recovery rate and adsorption capacity, and can meet the requirements of industrial production.
Description
Technical Field
The invention relates to the technical field of functional material preparation, in particular to a preparation method of a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode.
Background
The uranium resources in China are deficient, the land uranium ores are low in grade, and a plurality of depleted uranium ores exist, so that the nuclear fuel supply requirement in China in the future is difficult to meet. The uranium is efficiently separated from the uranium-containing waste liquid, so that the uranium resource can be effectively recycled, and the environmental pollution can be favorably reduced. By conventional separation methods, e.g. solvent extractionMembrane separation and the like are used for separating and enriching low-concentration uranium, and the technical and economic feasibility of the method is poor; the electro-adsorption is an effective method for separating uranium from uranium-containing wastewater, and has the advantages of low energy consumption, low pollution, economy and high efficiency. The adsorption capacity of the conventional adsorbent to U (VI) is more than tens of mg/g, and the U (VI) adsorption capacity can be improved by times by utilizing the electric adsorption; and by applying reverse potential to the working electrode, U (VI) is easy to desorb, thereby avoiding using a large amount of acidic desorption liquid; the method can also remove anions (such as NO) in the solution while separating U (VI) by using electric adsorption3-) that trap both simultaneously within the porous media of the counter electrode, also in preference to conventional adsorbents.
The key point of the electric adsorption separation of uranium in wastewater lies in the development of a novel efficient electrode material, and a carbon material has good corrosion resistance and stability and is a common electric adsorption electrode material. The carbon aerogel has the advantages of developed porous structure, good chemical stability, high specific surface area and large adsorption capacity, so that the carbon aerogel is an electrode material with good electric adsorption. Chemical products such as polyhydric alcohol, acid and the like are used as raw materials to prepare the carbon aerogel, but the production cost is high; the carbon aerogel can also be prepared by a template-oriented method, but the process is complex, depends on the fine structure and the size of the template, and is difficult to produce in batches. Therefore, how to prepare the high-performance electrode material at low cost is the key point for separating uranium from uranium-containing wastewater by utilizing electric adsorption.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode, so as to solve the problems in the background art.
The technical problem solved by the invention is realized by adopting the following technical scheme:
the preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode comprises the following specific steps:
(1) preparation of Biomass source N, P Co-doped carbon aerogel
Removing outer skins of waste biomass (such as shaddock peel, sugarcane hawthorn and the like), cutting into a proper size, cleaning, fully absorbing water in the cleaned biomass, adding the cleaned biomass, deionized water and N, P co-doping sources into a hydrothermal kettle, carrying out hydrothermal reaction at the temperature of 250 ℃ to obtain pre-carbonized N, P co-doped carbohydrate gel, and further removing soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel;
finally, cutting the pre-carbonized N, P co-doped carbon aerogel without soluble impurities into small squares, freeze-drying at the temperature of-60 ℃ to form the small squares, and introducing protective gas to carbonize at the temperature of 700 ℃ for 4 hours to obtain N, P co-doped carbon aerogel;
(2) n, P co-doped carbon aerogel/chitosan composite membrane electrode preparation method
Adding a certain amount of chitosan into acetic acid, stirring until the chitosan is completely dissolved to obtain a chitosan solution, then adding N, P co-doped carbon aerogel obtained in the step (1) into the chitosan solution according to the mass ratio, mixing, adding a certain amount of cross-linking agent and conductive carbon black, fully and uniformly stirring to obtain viscous mixed liquid, finally uniformly coating the viscous mixed liquid on a titanium dioxide plate, and drying at the temperature of 120 ℃ to obtain the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode.
In the present invention, in step (1), the N, P co-doping source is aminomethylphosphonic acid.
In the invention, in the step (1), 30g of biomass, 80ml of deionized water and 3g of N and P co-doping source are added into the hydrothermal kettle.
In the invention, in the step (1), the hydrothermal reaction is carried out for 14-18 h.
In the present invention, in step (1), the procedure for removing soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel is as follows: the pre-carbonized N, P co-doped carbohydrate gel was soaked in a mixture of water and ethanol for several days.
In the present invention, in the step (2), the acetic acid concentration is 1 wt%.
In the invention, in the step (2), the mass ratio of the chitosan to the N, P co-doped carbon aerogel is 1: 0.1-0.3.
In the invention, in the step (2), the optimal mass ratio of the chitosan to the N, P co-doped carbon aerogel is 1: 0.2.
In the present invention, in the step (2), the conductive carbon black is 1.0 g.
In the invention, in the step (2), the crosslinking agent is epichlorohydrin, and the volume of the epichlorohydrin is 1.5 mL.
In the invention, in the step (2), the protective gas is N2。
Has the advantages that:
(1) according to the invention, cheap natural biomass which is a natural plant fiber sponge structure and is discarded in agricultural processing, such as shaddock peel and bagasse, is used as a raw material to prepare N, P co-doped carbon aerogel with a developed pore structure, and N, P co-doped carbon aerogel is further compounded with chitosan to prepare a N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode for electro-adsorption separation of uranium in uranium-containing wastewater, so that the production cost is reduced, and the material performance is improved;
(2) according to the invention, when the biological carbon aerogel is prepared, aminomethyl phosphonic acid is used as a co-doping N, P source, hybrid N, P atom is introduced into the carbon aerogel, and hybrid N, P atom with lone pair electrons can be used as Lewis alkali to effectively complex uranyl ions, so that the adsorption capacity of the electro-adsorption separation uranium is improved;
(3) according to the invention, N, P co-doped biomass carbon aerogel is compounded with chitosan to prepare the N, P co-doped carbon aerogel/crosslinked chitosan composite membrane electrode, the chitosan can improve the hydrophilicity of the carbon aerogel and introduce a new adsorption site, so that the uranium electro-adsorption separation effect is improved;
(4) the biomass source N, P co-doped carbon aerogel/chitosan composite membrane electrode prepared by the invention has high specific surface area, good conductivity and chemical stability, and has high uranium recovery rate and adsorption capacity when being used for electro-adsorption separation of uranium in uranium-containing wastewater, and can meet the requirements of industrial production.
Drawings
FIG. 1 is a schematic flow chart of the preferred embodiment of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to be understood and clear, the invention is further described by combining the specific embodiments.
Example 1 (implemented according to the mass ratio of chitosan to N, P co-doped carbon aerogel of 1: 0.1)
The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode comprises the following specific steps:
(1) preparation of Biomass source N, P Co-doped carbon aerogel
Removing outer skins of waste biomass (shaddock peel and bagasse), cutting into a proper size, washing, fully absorbing water of 30g of biomass, adding the biomass, 80ml of deionized water and 3g of aminomethylphosphonic acid (N, P co-doping source) into a hydrothermal kettle, carrying out hydrothermal reaction for 16h at the temperature of 250 ℃ to obtain pre-carbonized N, P co-doped carbohydrate gel, and soaking the pre-carbonized N, P co-doped carbohydrate gel in a mixed solution consisting of water and ethanol for several days to remove soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel;
finally, cutting the pre-carbonized N, P co-doped carbohydrate gel without soluble impurities into small blocks, freeze-drying the small blocks at the temperature of-60 ℃ to form the small blocks, and introducing N at the temperature of 700 DEG C2Carbonizing the protective gas for 4 hours to obtain N, P co-doped carbon aerogel;
(2) n, P co-doped carbon aerogel/chitosan composite membrane electrode preparation method
Adding 10.0g of chitosan into 1 wt% of acetic acid, stirring until the chitosan is completely dissolved to obtain a chitosan solution, then adding 1.0g of N and P co-doped carbon aerogel obtained in the step (1) into the chitosan solution for mixing, adding 1.5 g of 1.5m L epoxy chloropropane cross-linking agent and 1.0g of conductive carbon black, fully and uniformly stirring to obtain a viscous mixed solution, finally uniformly coating the viscous mixed solution on a titanium dioxide plate, and drying at the temperature of 120 ℃ to prepare a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode (the thickness of the membrane is controlled by a fractional coating);
the electric adsorption device comprises an electric adsorption pool, a pH meter, a conductivity meter and a direct-current power supply, wherein a working electrode is an N, P co-doped carbon aerogel/chitosan composite membrane electrode (a 10 multiplied by 10mm membrane) bonded with a titanium dioxide plate, the prepared N, P co-doped carbon aerogel/chitosan composite membrane electrode is used as the working electrode, a conductive carbon membrane with the same size is used as a counter electrode, the potential of the working electrode is controlled to be-0.9V, uranium tailing wastewater (U (VI) with the concentration of 7.5mg/L) is used as a water sample, the feeding flow rate is controlled to be 1L/h, and continuous electric adsorption is carried out for 50 h.
Example 2 (implemented with a mass ratio of chitosan to N, P co-doped carbon aerogel of 1: 0.2)
The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode comprises the following specific steps:
(1) preparation of Biomass source N, P Co-doped carbon aerogel
Removing outer skins of waste biomass (shaddock peel and bagasse), cutting into a proper size, washing, fully absorbing water of 30g of biomass, adding the biomass, 80ml of deionized water and 3g of aminomethylphosphonic acid (N, P co-doping source) into a hydrothermal kettle, carrying out hydrothermal reaction for 16h at the temperature of 250 ℃ to obtain pre-carbonized N, P co-doped carbohydrate gel, and soaking the pre-carbonized N, P co-doped carbohydrate gel in a mixed solution consisting of water and ethanol for several days to remove soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel;
finally, cutting the pre-carbonized N, P co-doped carbohydrate gel without soluble impurities into small blocks, freeze-drying the small blocks at the temperature of-60 ℃ to form the small blocks, and introducing N at the temperature of 700 DEG C2Carbonizing the protective gas for 4 hours to obtain N, P co-doped carbon aerogel;
(2) n, P co-doped carbon aerogel/chitosan composite membrane electrode preparation method
Adding 10.0g of chitosan into 1 wt% acetic acid, stirring until the chitosan is completely dissolved to obtain a chitosan solution, then adding 2.0g of N and P co-doped carbon aerogel obtained in the step (1) into the chitosan solution for mixing, adding 1.5mL of epoxy chloropropane cross-linking agent and 1.0g of conductive carbon black, fully stirring to obtain a viscous mixed solution, finally uniformly coating the viscous mixed solution on a titanium dioxide plate, and drying at 120 ℃ to prepare a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode (the thickness of the membrane is controlled by fractional coating);
the electric adsorption device comprises an electric adsorption tank, a pH meter, a conductivity meter and a direct-current power supply, wherein a working electrode is an N, P co-doped carbon aerogel/chitosan composite membrane electrode (a 10 x 10mm membrane) bonded with a titanium dioxide plate, the prepared N, P co-doped carbon aerogel/chitosan composite membrane electrode is used as the working electrode, a conductive carbon membrane with the same size is used as a counter electrode, the potential of the working electrode is controlled to be-0.9V, the electric adsorption time is 1h, the uranium tailing wastewater (U (VI) concentration is 7.5mg/L) is used as a water sample, the feeding flow rate is controlled to be 1L/h, and continuous electric adsorption is performed for 50h, and the result shows that the U (VI) extraction rate is 98% and the uranium adsorption capacity is 367.5 mg/g.
Example 3 (implemented with a mass ratio of chitosan to N, P co-doped carbon aerogel of 1: 0.3)
The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode comprises the following specific steps:
(1) preparation of Biomass source N, P Co-doped carbon aerogel
Removing outer skins of waste biomass (shaddock peel and bagasse), cutting into a proper size, washing, fully absorbing water of 30g of biomass, adding the biomass, 80ml of deionized water and 3g of aminomethylphosphonic acid (N, P co-doping source) into a hydrothermal kettle, carrying out hydrothermal reaction for 16h at the temperature of 250 ℃ to obtain pre-carbonized N, P co-doped carbohydrate gel, and soaking the pre-carbonized N, P co-doped carbohydrate gel in a mixed solution consisting of water and ethanol for several days to remove soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel;
finally, cutting the pre-carbonized N, P co-doped carbohydrate gel without soluble impurities into small blocks, freeze-drying the small blocks at the temperature of-60 ℃ to form the small blocks, and introducing N at the temperature of 700 DEG C2Carbonizing the protective gas for 4 hours to obtain N, P co-doped carbon aerogel;
(2) n, P co-doped carbon aerogel/chitosan composite membrane electrode preparation method
Adding 10.0g of chitosan into 1 wt% acetic acid, stirring until the chitosan is completely dissolved to obtain a chitosan solution, then adding 3.0g of N and P co-doped carbon aerogel obtained in the step (1) into the chitosan solution for mixing, adding 1.5mL of epoxy chloropropane cross-linking agent and 1.0g of conductive carbon black, fully stirring to obtain a viscous mixed solution, finally uniformly coating the viscous mixed solution on a titanium dioxide plate, and drying at 120 ℃ to prepare a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode (the thickness of the membrane is controlled by fractional coating);
the electric adsorption device comprises an electric adsorption cell, a pH meter, a conductivity meter and a direct-current power supply, wherein a working electrode is an N, P co-doped carbon aerogel/chitosan composite membrane electrode (a 10 x 10mm membrane) bonded with a titanium dioxide plate, the prepared N, P co-doped carbon aerogel/chitosan composite membrane electrode is used as the working electrode, a conductive carbon membrane with the same size is used as a counter electrode, the potential of the working electrode is controlled to be-0.9V, the electric adsorption time is 1h, the uranium tailing wastewater (U (VI) concentration is 7.5mg/L) is used as a water sample, the feeding flow rate is controlled to be 1L/h, and continuous electric adsorption is performed for 50h, and the result shows that the U (VI) extraction rate is 84%, and the uranium adsorption capacity reaches 315 mg/g.
The results of the test on the N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode prepared in examples 1 to 3 for the electro-adsorption separation of uranium in wastewater show that: when the mass ratio of the chitosan to the N, P co-doped carbon aerogel is 1:0.2, the prepared N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode has the best effect on separating uranium in wastewater; when N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode is prepared, the amount of chitosan is properly increased, which is beneficial to improving the uranium electro-adsorption separation effect (as compared with example 2 and example 3, the effect of example 2 is better), because chitosan can improve the hydrophilicity of carbon aerogel and introduces an amino adsorption site; however, if the amount of chitosan is too high, the carbon material pores are blocked, and the adsorption in the uranium inlet holes is not facilitated, so that the performance of uranium electroadsorption separation is affected, and the uranium adsorption capacity is reduced (as compared with example 1 and example 2, the effect of example 1 is poor).
Claims (10)
1. The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode is characterized by comprising the following specific steps:
(1) preparation of Biomass source N, P Co-doped carbon aerogel
Removing the outer skin of the waste biomass, cutting into a proper size, cleaning, fully absorbing water in the cleaned biomass, adding the cleaned biomass, deionized water and N, P co-doping source into a hydrothermal kettle, carrying out hydrothermal reaction at the temperature of 250 ℃ to obtain pre-carbonized N, P co-doped carbohydrate gel, and further removing soluble impurities in the pre-carbonized N, P co-doped carbohydrate gel;
finally, cutting the pre-carbonized N, P co-doped carbon aerogel without soluble impurities into small squares, freeze-drying at the temperature of-60 ℃ to form the small squares, and introducing protective gas to carbonize at the temperature of 700 ℃ for 4 hours to obtain N, P co-doped carbon aerogel;
(2) n, P co-doped carbon aerogel/chitosan composite membrane electrode preparation method
Adding a certain amount of chitosan into acetic acid, stirring until the chitosan is completely dissolved to obtain a chitosan solution, then adding N, P co-doped carbon aerogel obtained in the step (1) into the chitosan solution according to the mass ratio, mixing, adding a certain amount of cross-linking agent and conductive carbon black, fully and uniformly stirring to obtain viscous mixed liquid, finally uniformly coating the viscous mixed liquid on a titanium dioxide plate, and drying at the temperature of 120 ℃ to obtain the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode.
2. The method for preparing the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 1, wherein in step (1), the N, P co-doped source is aminomethylphosphonic acid.
3. The method for preparing the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode as claimed in claim 1, wherein in step (1), 30g of biomass, 80ml of deionized water and 3g of N and P co-doped sources are added into the hydrothermal kettle.
4. The method for preparing the biomass source N, P codoped carbon aerogel/crosslinked chitosan composite membrane electrode of claim 1, wherein the procedure for removing soluble impurities in the pre-carbonized N, P codoped carbohydrate gel in step (1) is as follows: the pre-carbonized N, P co-doped carbohydrate gel was soaked in a mixture of water and ethanol for several days.
5. The method for preparing a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 1, wherein in step (2), the acetic acid concentration is 1 wt%.
6. The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 1, wherein in the step (2), the mass ratio of the chitosan to the N, P co-doped carbon aerogel is 1: 0.1-0.3.
7. The preparation method of the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 6, wherein in the step (2), the optimal mass ratio of the chitosan to the N, P co-doped carbon aerogel is 1: 0.2.
8. The method for preparing a biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 1, wherein in step (2), the amount of conductive carbon black is 1.0 g.
9. The method for preparing the biomass source N, P co-doped carbon aerogel/crosslinked chitosan composite membrane electrode of claim 1, wherein in step (2), the crosslinking agent is epichlorohydrin, and the amount of epichlorohydrin is 1.5 mL.
10. The method for preparing the biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode of claim 1, wherein in the step (2), the protective gas is N2。
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| CN113582300A (en) * | 2021-08-05 | 2021-11-02 | 核工业北京化工冶金研究院 | Method for removing uranium element in water through electro-adsorption |
| CN113816473A (en) * | 2021-10-28 | 2021-12-21 | 辽宁大学 | Method for combined electrically enhanced adsorption of Re (VII) by mushroom rod-based conductive composite aerogel |
| CN114082399A (en) * | 2021-10-15 | 2022-02-25 | 东华理工大学 | Uranium adsorbent based on N, P-doped porous carbon material and preparation method thereof |
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