CN113003675A - Mxene material with organic chelating functional group grafted on surface and preparation method thereof - Google Patents
Mxene material with organic chelating functional group grafted on surface and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of Mxene material modification, and discloses an Mxene material with a surface grafted with an organic chelating functional group. The invention also discloses a preparation method of the Mxene material, which comprises the following steps: s1, dispersing Mxene powder in an organic solvent to obtain a suspension I, and adding a grafting agent into the organic solvent to obtain a solution II; and S2, adding the solution II into the suspension I, stirring and reacting under the ultrasonic condition, separating out a solid, and washing and drying to obtain the product. The preparation process is controllable and simple, the operation is simple and convenient, the material has good shape and structure, the number of the chelated functional groups grafted on the surface is considerable and uniform, and the material is used as a capacitive deionization electrode material and has excellent performance of removing heavy metal ions and radioactive ions, so that the high-efficiency treatment of water is realized, the material can be regenerated and recycled, and the preparation method has large-scale industrial production and application prospects.
Description
Technical Field
The invention belongs to the field of Mxene material modification, and particularly relates to an Mxene material with a surface grafted with an organic chelating functional group and a preparation method thereof.
Background
Since the stepping of human beings into industrial society and the development and application of nuclear energy, the pollution of heavy metals and radioactive ions has been an environmental problem seriously threatening the health and ecological environment of human beings. How to effectively treat the industrial pollution is always the subject focus of researchers. Although many traditional methods are developed to treat heavy metal and radioactive ion pollution at present, the methods all face practical application problems, such as low efficiency, poor effect on low-concentration ions, secondary pollution caused by treatment substances, incapability of regeneration, high cost and the like. Therefore, the development of a novel treatment strategy is particularly urgent.
Capacitive Deionization (CDI) is a novel water treatment technology that is efficient, environmentally friendly, simple to operate, and economical. At present, the method is applied to desalination and water body softening on a large scale. Based on the previous research results, the treatment of heavy metals and radioactive ions by CDI can also have good effect. However, heavy metals and radioactive ions are different from light sodium, calcium, magnesium and the like ions in desalination and softening, and accordingly, electrodes which are key core components of CDI need to be designed and prepared specifically, and the key of the electrodes is active electrode materials. Therefore, the key point of the technology is to design an electrode material aiming at treating heavy metal and radioactive ions.
Mxene has received extensive research and attention as a new two-dimensional material since 2011. Due to the unique layered structure and crystal structure, Mxene can be used as an excellent electrode material for CDI. However, for the adsorption and treatment of heavy metals and radioactive ions, it is difficult to achieve efficient and complete removal by pure Mxene, and the pure Mxene is unstable in anchoring of these ions. Although there are reports of introducing active hydroxyl groups on the surface of Mxene for removing lead ions, the adsorption capacity of the material is limited, and the material cannot be regenerated and reused. Also at Ti3C2TxThe Mexne is loaded with nano silver particles for desalting, but silver is a noble metal, so the cost is high, and the large-scale application is not facilitated. Therefore, the cheap and efficient Mxene with modified surface functional groups is researched and developed to be applied toHeavy metal and radioactive ion treatment is particularly urgent.
Disclosure of Invention
The invention aims to provide a Mxene material with good conductivity, high adsorption capacity, high efficiency, and renewable and reusable surface grafted organic chelating functional groups.
The invention also aims to provide a preparation method of the Mxene material, which has simple process flow and simple and convenient operation and can realize industrialized production.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
an Mxene material with organic chelating functional groups grafted on the surface, wherein the Mxene material is combined with a grafting agent through a siloxane bond, and the grafting agent contains amino and/or carboxyl as the organic chelating functional groups.
Further, the Mxene material is Ti3C2。
Furthermore, the mesh number of the Mxene material is 200-800 meshes.
Further, the grafting agent is selected from at least one of N- (trimethoxysilylpropyl) ethylenediamine triacetic acid, N- (3-trimethoxysilylpropyl) ethylenediamine, N- (3-trimethoxysilylethyl) ethylenediamine, N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane and aminoethylaminoisobutylmethyldimethoxysilane.
The preparation method of the Mxene material comprises the following steps:
s1, dispersing Mxene powder in an organic solvent to obtain a suspension I, and adding a grafting agent into the organic solvent to obtain a solution II;
and S2, adding the solution II into the suspension I, stirring and reacting under the ultrasonic condition, separating out a solid, and washing and drying to obtain the product.
Further, the solid content of the suspension I is 1-10 g/L; the amount of Mxene added is 1-5 g as required.
Further, the concentration of the grafting agent of the solution II is 2-10 wt%; the amount of the grafting agent added is determined according to the requirement, and can be 100-500 mg.
Further, the volume ratio of the suspension I to the solution II in the S2 is 1: 0.01 to 0.1.
Further, the organic solvent is ethanol or methanol.
Further, the cleaning is sequentially performed by using a cleaning solvent and water, wherein the cleaning solvent is at least one of methanol, ethanol, ethylene glycol, acetone and toluene.
Further, the reaction temperature in the S2 is 50-80 ℃, and the reaction time is 5-15 h.
The invention has the following beneficial effects:
the surface of the Mxene material is grafted with a large number of organic chelating functional groups (amino and carboxyl) through covalent bonds, the chelating functional groups can strongly anchor heavy metal ions (such as lead, mercury, cadmium and strontium) and radioactive ions (such as cesium) in polluted water, and the adsorption capacity can reach 210mg g-1The removal efficiency can reach 99%, and the adsorption rate is very fast (5min is close to equilibrium). The chelating functional group grafted on the surface of the Mxene has strong capturing capacity for heavy metal ions, and can serve as an adsorption active site on the surface of the Mxene to improve the surface adsorption activity of the Mxene, so that the adsorption capacity, the removal efficiency and the adsorption kinetics are improved. In contrast, the Mxene without the chelating functional group modification had half the adsorption capacity of the Mxene material of the invention and the removal efficiency was less than 90%.
The Mxene material adopted by the invention has numerous and uniform hydroxyl functional groups on the surface in the etching preparation process, and can provide adsorption active sites for grafting the chelating functional groups, one end of the grafting agent is provided with a silane functional group, and the functional group can generate polymerization reaction with the hydroxyl on the Mxene surface after hydrolysis to form stable silicon-oxygen bonds, so that the chelating functional groups are grafted to the Mxene surface.
The Mxene material can realize complete removal and regeneration in an external reverse electric field, thereby realizing efficient recycling. The external reverse electric field can give a strong driving force to the metal ions, so that the chelate bonds are broken after the metal ions are activated, and the regeneration of the material is realized. The regeneration process does not need acid washing, so no secondary pollution is generated. While the use of Mxene materials for heavy metal adsorption does not result in such regeneration capability.
The preparation process is controllable and simple, the operation is simple and convenient, the material has good shape and structure, the number of the chelated functional groups grafted on the surface is considerable and uniform, and the material is used as a capacitive deionization electrode material and has excellent performance of removing heavy metal ions and radioactive ions, so that the high-efficiency treatment of water is realized, the material can be regenerated and recycled, and the preparation method has large-scale industrial production and application prospects.
Drawings
FIG. 1 is an SEM image of a Mxene material with organic chelating functional groups grafted on the surface of the Mxene material in example 1;
FIG. 2 is an XRD pattern of Mxene material with organic chelating functional groups grafted on the surface of the Mxene material in example 1;
FIG. 3 is a FTIR plot of Mxene material surface grafted with organochelating functionality according to example 1;
FIG. 4 is an adsorption isotherm of a Mxene material surface grafted with an organic chelating functional group of example 1;
FIG. 5 is a graph of the regeneration mechanism of the Mxene material with the surface grafted with organic chelating functional groups of example 1.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
Mxene material grafted with organic chelating functional group is prepared according to the following steps
S1, mixing 1g of Ti with 400 meshes3C2Dispersing the powder in 200mL of ethanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 5g/L), adding 200mg of N- (trimethoxysilylpropyl) ethylenediamine triacetic acid into 10mL of ethanol to obtain a solution II (2.47 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.05, performing ultrasonic treatment and stirring to mix uniformly, performing stirring reaction for 12 hours at 65 ℃, then performing centrifugal separation to obtain a black solid, washing with ethanol and water, and drying in an air-blast drying oven at 80 ℃ for 12 hours to obtain a final product.
FIG. 1 is an SEM image of a Mxene material, which can be seen to be in the shape of a louver formed by stacking two-dimensional nanosheets;
FIG. 2 is an XRD pattern of Mxene material showing that Mxene crystallizes well with substantially no other hetero-phases present;
FIG. 3 is an FTIR plot of Mxene material at 3400cm-1A stretching vibration peak of hydroxyl appears, which proves that the ethylenediamine-triethyl acid chain (the organic chelating functional group of which is carboxyl) is successfully grafted to the surface of Mxene;
200mg of Mxene material is made into an electrode, and is used for CDI to adsorb solution with concentration of 50ppm and 200mL and containing heavy metal ions or radioactive ions (such as lead, mercury, cadmium, strontium, cesium and the like), the concentration of residual copper ions is tested after 1h, and the residual copper ions are divided by the initial concentration to obtain the removal efficiency. The adsorption capacity can be tested by reference to the methods of the prior art (e.g., environ. sci.: Nano,2017,4, 1114-1123), and the adsorption time is 5 min.
FIG. 4 is a cesium ion adsorption isotherm for a Mxene material, which can be seen to have a cesium ion adsorption capacity of 210mg g-1The removal efficiency was 99.6%.
Comparative experiment: mxene modified without chelating functional group and having an adsorption capacity of 99.8mg g-1The removal efficiency was 86.4%.
FIG. 5 is a graph of the regeneration mechanism of Mxene materials by slowly applying a voltage from 0V to 1.6V and then slowly decreasing the voltage to-1.4V, and monitoring the solution concentration and calculating the adsorption capacity in real time. The experiment shows that almost all adsorbed cesium ions can be reversibly removed under the voltage of-1.4V, only a reverse electric field is needed to be added in the process, acid washing desorption is not needed, secondary pollution is avoided, and the method is convenient and rapid.
Example 2
The Mxene material grafted with organochelating functionality was prepared according to the following procedure:
s1, mixing 1g of Ti with 400 meshes3C2Dispersing the powder in 200mL of ethanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 5g/L), adding 300mg of N- (3-trimethoxysilylethyl) ethylenediamine into 10mL of ethanol to obtain a solution II (3.66 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.05, performing ultrasonic treatment and stirring to mix uniformly, performing stirring reaction for 12 hours at 65 ℃, then performing centrifugal separation to obtain a black solid, washing with ethanol and water, and drying in an air-blast drying oven at 80 ℃ for 12 hours to obtain a final product.
The effective chelating functional group grafted on the surface of the Mxene material of the embodiment is amino, and the Mxene material can effectively chelate and remove heavy metal ions as a CDI electrode material. An adsorption experiment was carried out by referring to the method of example 1, and the lead adsorption capacity was 310.3mg g-1The removal efficiency was 99.5%.
Comparative experiment: mxene modified without chelating functional groups and having an adsorption capacity of 152.3mg g-1The removal efficiency was 83.9%.
Example 3
The Mxene material grafted with organochelating functionality was prepared according to the following procedure:
s1, mixing 1g of Ti with 800 meshes3C2Dispersing the powder in 200mL of ethanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 5g/L), adding 400mg of N- (3-trimethoxysilylpropyl) ethylenediamine into 10mL of ethanol to obtain a solution II (4.83 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.05, performing ultrasonic treatment and stirring to mix uniformly, performing stirring reaction for 10 hours at 75 ℃, then performing centrifugal separation to obtain black solid, washing with methanol and water, and drying in an air-blast drying oven at 80 ℃ for 12 hours to obtain the final product.
The Mxene material of the embodiment has excellent efficiency of removing the chelate of heavy metal ions and is reproducible, and the adsorption experiment is carried out according to the method of the embodiment 1, and the capacity of adsorbing copper ions is 75.6mg g-1The removal efficiency was 99.0%.
Comparative experiment: mxene modified without chelating functional group and having an adsorption capacity of 32.1mg g-1The removal efficiency was 88.3%.
Example 4
The Mxene material grafted with organochelating functionality was prepared according to the following procedure:
s1, mixing 3g,200 mesh Ti3C2Dispersing the powder in 3000mL of methanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 1g/L), adding 100mg of grafting agent N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane into 1.2mL of methanol to obtain a solution II (9.54 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.1, performing ultrasonic treatment and stirring to mix uniformly, performing stirring reaction for 15h at 55 ℃, then performing centrifugal separation to obtain black solids, washing with acetone and water, and drying in an air-blast drying oven at 80 ℃ for 12h to obtain the final product.
An adsorption experiment was carried out by referring to the method of example 1, and the capacity for adsorbing copper was 85.2mg g-1The removal efficiency was 99.4%.
Comparative experiment: mxene modified without chelating functional group and having an adsorption capacity of 35.1mg g-1The removal efficiency was 89.3%.
Example 5
The Mxene material grafted with organochelating functionality was prepared according to the following procedure:
s1, mixing 5g of Ti with 600 meshes3C2Dispersing the powder in 500mL of ethanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 10g/L), adding 500mg of a grafting agent aminoethylaminoisobutylmethyldimethoxysilane into 10mL of ethanol to obtain a solution II (5.96 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.01, performing ultrasonic treatment, stirring and mixing uniformly, performing stirring reaction for 8 hours at the temperature of 80 ℃, then performing centrifugal separation to obtain black solids, washing with ethylene glycol and water, and drying in an air-blast drying oven at the temperature of 80 ℃ for 12 hours to obtain a final product.
An adsorption experiment was carried out by referring to the method of example 1, and the lead adsorption capacity was 325mg g-1The removal efficiency was 99.4%.
Comparative experiment: mxene modified without chelating functional group and having lead adsorption capacity of 152mg g-1The removal efficiency was 88.5%.
Example 6
The Mxene material grafted with organochelating functionality was prepared according to the following procedure:
s1, mixing 4g of Ti with 400 meshes3C2Dispersing the powder in 500mL of ethanol by ultrasonic and magnetic stirring to obtain a suspension I (the solid content is 8g/L), adding 250mg of grafting agent N- (3-trimethoxysilylpropyl) ethylenediamine into 3.5mL of ethanol to obtain a solution II (8.30 wt%), and uniformly mixing for later use;
s2, adding the solution II into the suspension I, wherein the volume ratio of the suspension I to the solution II is 1: 0.03, performing ultrasonic treatment and stirring to mix uniformly, performing stirring reaction for 5 hours at 50 ℃, then performing centrifugal separation to obtain black solids, washing with toluene and water, and drying in an air-blast drying oven at 80 ℃ for 12 hours to obtain the final product.
An adsorption experiment was carried out by referring to the method of example 1, and the adsorption capacity of cesium was 196.3mg g-1The removal efficiency was 99.5%.
Comparative experiment: mxene modified without chelating functional group and having cesium adsorption capacity of 85.8mg g-1The removal efficiency was 85.8%.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An Mxene material with a surface grafted with an organic chelating functional group is characterized in that the Mxene material is combined with a grafting agent through a silicon-oxygen bond, and the grafting agent contains an amino group and/or a carboxyl group as the organic chelating functional group.
2. An Mxene material according to claim 1, wherein the Mxene material is Ti3C2。
3. A Mxene material according to claim 2, characterized in that the mesh number of the Mxene material is 200-800 meshes.
4. A Mxene material according to claim 1 or 2, wherein the grafting agent is selected from at least one of N- (trimethoxysilylpropyl) ethylenediamine triacetic acid, N- (3-trimethoxysilylpropyl) ethylenediamine, N- (3-trimethoxysilylethyl) ethylenediamine, N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane, aminoethylaminoisobutylmethyldimethoxysilane.
5. A method of preparing a Mxene material as claimed in any of claims 1 to 4, which comprises the steps of:
s1, dispersing Mxene powder in an organic solvent to obtain a suspension I, and adding a grafting agent into the organic solvent to obtain a solution II;
and S2, adding the solution II into the suspension I, stirring and reacting under the ultrasonic condition, separating out a solid, and washing and drying to obtain the product.
6. The process according to claim 5, wherein the suspension I has a solids content of 1 to 10g/L and the solution II has a grafting agent concentration of 2 to 10 wt.%.
7. The method of claim 5, wherein the volume ratio of suspension I to solution II in S2 is 1: 0.01 to 0.1.
8. The method of claim 5, wherein the organic solvent is ethanol or methanol.
9. The method according to claim 5, wherein the washing is sequentially washing with a washing solvent and water, and the washing solvent is at least one of methanol, ethanol, ethylene glycol, acetone, and toluene.
10. The method according to claim 5, wherein the reaction temperature in S2 is 50-80 ℃ and the reaction time is 5-15 h.
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CN113426428A (en) * | 2021-06-28 | 2021-09-24 | 武汉大学 | Polyaniline-sulfur nitrogen MXene/sodium alginate composite gel adsorbent and preparation method and application thereof |
CN114160091A (en) * | 2021-12-02 | 2022-03-11 | 东北林业大学 | Preparation method of hydroxyl functionalized titanium carbide and application of hydroxyl functionalized titanium carbide in efficient adsorption and cesium removal |
CN114455690A (en) * | 2021-12-23 | 2022-05-10 | 南京师范大学 | Magnetic Mxene microbial carrier material and preparation method thereof |
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CN113426428A (en) * | 2021-06-28 | 2021-09-24 | 武汉大学 | Polyaniline-sulfur nitrogen MXene/sodium alginate composite gel adsorbent and preparation method and application thereof |
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CN114160091A (en) * | 2021-12-02 | 2022-03-11 | 东北林业大学 | Preparation method of hydroxyl functionalized titanium carbide and application of hydroxyl functionalized titanium carbide in efficient adsorption and cesium removal |
CN114503982A (en) * | 2021-12-10 | 2022-05-17 | 南京师范大学 | MXexe- (g) -CP pesticide dispersant and preparation method thereof |
CN114503982B (en) * | 2021-12-10 | 2022-11-25 | 南京师范大学 | MXene- (g) -CP pesticide dispersant and preparation method thereof |
CN114455690A (en) * | 2021-12-23 | 2022-05-10 | 南京师范大学 | Magnetic Mxene microbial carrier material and preparation method thereof |
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