CN113083213B - Single-layer MXene colloid and preparation method and application thereof - Google Patents
Single-layer MXene colloid and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a monolayer MXene colloid and a preparation method and application thereof, wherein the method comprises the following steps: s1, dissolving anhydrous LiCl in inorganic acid to obtain a solution A; s2, adding MXene precursor into the solution A, and reacting at 50-60 ℃; s3, adding the reaction solution of S2 into a hydrochloric acid solution for reaction; after the reaction is finished, repeatedly adding water into the lower-layer precipitate for centrifugation until the pH value of the upper-layer clarified liquid is 5; s4, adding ethanol into the lower-layer precipitate of the S3, and carrying out ultrasonic treatment and separation; then collecting the lower-layer precipitate, adding water, performing ultrasonic treatment and separation, and collecting the upper-layer liquid to obtain a single-layer MXene colloid. The monolayer MXene colloid is applied to selective adsorption of uranyl ions. The method is simple to operate, and the prepared monolayer MXene colloid has good stability and high-efficiency selective uranyl removal performance.
Description
Technical Field
The invention relates to the technical field of MXene materials and uranyl wastewater treatment, in particular to a single-layer MXene colloid and a preparation method and application thereof.
Background
MXene is a novel two-dimensional structural material cooperatively discovered in 2011 by Gogotsi and Barsum et al, Derasel University (Drexel University) in USA. MAX phase material (ternary laminated ceramic) is used as a precursor, and a chemical etching method is used for removing the atomic layer with weaker combination in the MAX phase, so that MXene with a laminated structure can be prepared. Since the new material comes out, the material has received wide attention from researchers in the research fields of electrochemistry, functional nano materials and the like.
The general chemical formula of MXene can be M n+1 X n T z Represents; wherein M is a transition metal, e.g. Ti, Zr, HfV, Nb, Ta, Cr, Sc, etc.; x represents C or/and N; n is generally from 1 to 3; t is z Refers to surface groups, e.g. O 2- 、OH - 、F - 、NH 3 、NH 4 + And the like. It has a unique two-dimensional layered structure, and this type of graphene structure provides a diffusion channel for the intercalation/deintercalation of ions. However, as with other two-dimensional materials, the layered structure of MXene also brings a series of problems, such as greatly reducing the utilization rate of the specific surface area due to layer stacking, and greatly restricting the performance of MXene due to problems such as stacking and agglomeration, thereby severely limiting their application in many fields.
Until now, the application research of MXene materials mainly focuses on the field of energy materials, which are mainly combined with the high specific surface area, high conductivity, good electrolyte wettability, strong tensile and compressive capacities and high density (3.7 g/cm) of MXene materials 3 ) In connection with the preparation method, the material can be used as an electrode material of a super capacitor to show excellent electrochemical performance. In view of the unique surface physicochemical characteristics, MXene is also an adsorption material with excellent performance.
Further using NaOH intercalation activation treatment to prepare Ti on the basis of HF etching MAX phase material in Yanshan university Penqiming and the like 3 C 2 T x (T ═ OH/ONa, F) sheet material and its use for the adsorption of heavy metal ions Pb (II) in aqueous solutions and of other divalent competitive ions (Ca) 2+ ，Mg 2+ ) Preferential adsorption of Pb (II) in the presence of (J.Am.chem.Soc.2014, 136, 4113)]. Some researchers will use Ti 3 C 2 T x The lamellar material is used for researching the adsorption and photocatalytic degradation behaviors of dye molecules, such as adsorption of cationic dye molecule methyl orange by Mashtalir and the like [ J.Mater.chem.A 2014,2,14334]. Compared with heavy metal ions released by common industrial pollution, radioactive waste liquid generated by the nuclear industry has more obvious harm to human and natural environment. The maximum adsorption capacity of MXene material to radioactive palladium in solution reaches 184mg/g, and the material has good reusability [ chem]. How to improve MXene content in solution by structural modificationThe absorption performance of harmful nuclides is the current hot research topic [ chem. Eng.J.2020,397,1254282]。
Disclosure of Invention
In order to solve the problems, the invention aims to provide a monolayer MXene colloid, a preparation method thereof and application thereof in removing uranyl ions in wastewater through efficient selective adsorption.
In order to achieve the above object, the technical solution of the present invention is as follows.
A preparation method of single-layer MXene colloid comprises the following steps:
s1, dissolving anhydrous LiCl in inorganic acid to obtain a solution A;
s2, adding MXene precursor into the solution A, and reacting at 50-60 ℃;
s3, adding the reaction solution of S2 into a hydrochloric acid solution for reaction; after the reaction is finished, repeatedly adding water into the lower-layer precipitate for centrifugation until the pH value of the upper-layer clarified liquid is 5;
s4, adding ethanol into the lower-layer precipitate of the S3, and carrying out ultrasonic treatment and separation; then collecting the lower-layer precipitate, adding water, performing ultrasonic treatment and separation, and collecting the upper-layer liquid to obtain a single-layer MXene colloid.
Further, in S1, the inorganic acid is hydrofluoric acid and/or hydrochloric acid. Here, the mass concentration of hydrofluoric acid is about 40%; the mass concentration of the hydrochloric acid is about 36-37%.
Furthermore, in S1, the ratio of LiCl to inorganic acid is 1 g: 10-20 mL.
Further, in S2, the MXene precursor is Ti 3 AlC 2 、Ti 2 AlC、V 2 AlC、Nb 2 Any one or a mixture of more of AlC.
Furthermore, in S2, the mass ratio of the MXene precursor to LiCl is 1: 1 to 2.
Further, in S3, the dosage ratio of MXene precursor to hydrochloric acid solution is 1 g: 30 mL; the mass concentration of the hydrochloric acid solution is 18%.
Further, in S4, the solution before ultrasonic treatment needs to be treated by introducing nitrogen for 20 min; the ultrasonic process is carried out in an ice bath at 0-4 ℃; the ultrasonic time is 20-90 min. The ultrasonic is a 750W high-power ultrasonic machine.
Further, in S4, the ratio of the MXene precursor to the deionized water was 1 g: 20-60 mL. The final concentration of MXene colloid was controlled according to the amount of deionized water.
In S4, the ratio of MXene precursor to ethanol used in the reaction mixture is 1 g: 40-80 mL.
The invention also provides the single-layer MXene colloid prepared by the method.
The invention also provides an application of the single-layer MXene colloid in selective adsorption removal of uranyl ions.
The invention has the beneficial effects that:
1. the method mainly etches a few layers of MXene aggregates in HF/LiCl solution, and generates a single layer of MXene colloid through further ultrasonic treatment. The method provided by the invention has the advantages that the used equipment is simple, the prepared single-layer MXene colloid has good stability, large transverse area and high dispersity.
2. The single-layer MXene colloid prepared by the method has good selective adsorption performance on uranium milling. The electron microscopic analysis and the small-angle scattering technology show that the prepared single-layer MXene colloid has a monolithic layer structure and a high specific surface area, and has a negative surface potential, so that the single-layer MXene colloid has high adsorption efficiency on uranyl ions. X-ray photoelectron spectroscopy analysis shows that the redox property and the surface-F functional group of the monolayer MXene colloid are the essential reasons for selective adsorption of uranyl.
Drawings
FIG. 1 shows a single Ti layer obtained in example 1 of the present invention 3 C 2 T X Transmission electron microscopy images of colloids.
FIG. 2 is a bar graph comparing the adsorption performance of the products of example 1, comparative example 1 and comparative example 2 of the present invention with respect to uranyl U (VI).
FIG. 3 shows a single Ti layer obtained in example 1 of the present invention 3 C 2 T X Adsorption performance of the colloid to uranyl U (VI).
FIG. 4 shows a single Ti layer obtained in example 1 of the present invention 3 C 2 T X The colloid has adsorption performance for uranium ore stock solution.
FIG. 5 shows a multilayer Ti obtained in comparative example 1 3 C 2 T X Powder and few Ti layers 3 C 2 T X Electron microscopy images of Li powder. Wherein FIG. 5(a) shows a multilayer Ti 3 C 2 T X Electron microscopy images of the powder; FIG. 5(b and c) shows a few Ti layers 3 C 2 T X Electron microscopy images of Li powder.
FIG. 6 shows a Ti layer having a small content obtained in comparative example 2 3 C 2 T X Li and Single layer Ti obtained in example 1 of the invention 3 C 2 T X Small angle scattering data of colloids.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Single-layer Ti 3 C 2 T X The preparation method of the colloid comprises the following steps:
s1, respectively weighing Ti 3 AlC 2 2.000g (200mesh) of powder, 2.211g of anhydrous LiCl and 30mL of an HF solution with the mass concentration of 40 wt%;
firstly, adding 30mL of HF solution with the mass concentration of 40% into a polytetrafluoroethylene bottle, adding 2.211g of anhydrous LiCl into the HF solution, and stirring and dissolving to obtain a solution A;
s2, slowly adding Ti into the solution A 3 AlC 2 Powder, the charging time is 1 min; after the addition was complete, the reaction was allowed to proceedPlacing the mixture on a magnetic stirrer, stirring for 30min, placing the stirred mixed solution in an oven, and setting the temperature of the oven to be 50-60 ℃ to react for 24-48 h;
s3, cooling the reacted mixed solution in an oven to room temperature, taking out, adding 60mL of HCl solution with the mass concentration of 18% into a plastic beaker, adding the cooled mixed solution into the HCl solution, and standing for 2-4 hours or longer;
s4, pouring out the HCl solution on the upper layer when the reactant in the cup is precipitated to the bottom, and adding the precipitate on the bottom of the cup into four centrifuge tubes respectively for later use;
s5, adding deionized water into the centrifuge tube, centrifuging at 6000rpm for 10min, and pouring out supernatant;
s6, repeating the step S5 until the pH value of the supernatant liquid is 5;
s7, adding 40mL of ethanol into the lower-layer precipitate of the S6, and carrying out ultrasonic treatment for 60min in an ice bath by using a 750W ultrasonic machine;
s8, centrifuging the solution after ultrasonic treatment for 10min at 6000rpm by using a high-speed centrifuge;
s9, collecting the centrifuged lower-layer precipitate, adding 20mL of deionized water, introducing nitrogen for 20min, performing ultrasonic treatment for 20min by using a 750W ultrasonic machine, centrifuging, and taking the black brown supernatant to obtain a single-layer Ti 3 C 2 T X And (3) colloid. Wherein, T X mainly-F, -OH and a small amount of-Cl.
The monolayer Ti obtained above 3 C 2 T X The transmission electron micrograph of the gel is shown in FIG. 1.
The single layer Ti obtained above 3 C 2 T X The colloid is applied to selective adsorption of uranyl ions, and the specific operation is as follows:
1. adsorption experiment of uranyl nitrate
A single layer of Ti 3 C 2 T X And mixing the colloid with a certain amount of uranyl nitrate solution, and fixing the volume to 10mL together to prepare a mixed solution with a certain concentration gradient.
Monolayer of Ti in mixed solution 3 C 2 T X The concentration of the colloid was 0.05 mg/L.
The concentration range of uranyl nitrate is 0.02-2 mmol/L (gradient concentration values of uranyl nitrate are 0.02mmol/L, 0.04mmol/L, 0.12mmol/L, 0.2mmol/L, 0.28mmol/L, 0.36mmol/L, 0.50mmol/L, 0.80mmol/L, 1.12mmol/L and 2.00mmol/L respectively).
Centrifuging at 7000rpm for 3min after 24h, taking supernatant for dilution, testing the concentration of residual uranyl ions by using plasma inductively coupled emission spectroscopy, and calculating single-layer Ti 3 C 2 T X Adsorption capacity and adsorption partition coefficient K of colloid d . The adsorption performance results are shown in table 1 and fig. 3.
TABLE 1 Single layer Ti 3 C 2 T X Test result of adsorption performance of colloid on uranyl ions
From the results of table 1 and fig. 3, it is understood that the amount of adsorption of the single-layer MXene colloid increases as the concentration of uranyl nitrate increases, and the adsorption partition coefficient K increases d The adsorption tends to be saturated when the uranyl nitrate concentration is more than 1.2mmol/L, and the maximum adsorption capacity is 3.2mmol/g (the solid-liquid ratio is 1: 20000).
2. Competitive adsorption experiment of uranium ore stock solution
Taking a single layer of Ti 3 C 2 T X Mixing the colloid with uranium ore stock solution in a volume ratio of 1mL to 9mL, and carrying out single-layer Ti treatment on the mixed solution 3 C 2 T X The concentration of the colloid was 0.05 mg/L.
After 24h, centrifugation was carried out at 7000rpm for 3min, and then the supernatant was taken and diluted. Detecting the concentrations of uranyl ions and other cations in the solution before and after adsorption of the uranium ore stock solution by using plasma inductively coupled emission spectroscopy, detecting the change of the concentration of anions in the solution by using ion chromatography, and calculating the single-layer Ti 3 C 2 T X Selective adsorption properties of the colloid. The adsorption performance results are shown in fig. 4.
As can be seen from FIG. 4, there are a number of competing ions (Na) + ，Ca +2 ，Mg +2 ，Cl - ，SO 4 -2 ) Under the action of (2), a single layer of Ti 3 C 2 T X The colloid shows good selective adsorption performance on uranyl ions.
Example 2
Single-layer Ti 3 C 2 T X The colloid was prepared in substantially the same manner as in example 1, except that,
in S1, Ti is weighed respectively 3 AlC 2 2.000g (200mesh) of powder, 2.000g of anhydrous LiCl, and 40mL of a 40 wt% HF solution;
in S7, adding 60mL of ethanol into the lower-layer precipitate of S6, and carrying out ultrasonic treatment for 30min in an ice bath by using a 750W ultrasonic machine;
in S9, the lower precipitate after centrifugation was collected and 40mL of deionized water was added.
Example 3
Single-layer Ti 3 C 2 T X The colloid was prepared in substantially the same manner as in example 1, except that,
in S1, Ti is weighed respectively 3 AlC 2 2.000g (200mesh) of powder, 4.000g of anhydrous LiCl, and 40mL of a 40 wt% HF solution;
in S7, adding 80mL of ethanol into the lower-layer precipitate of S6, and carrying out ultrasonic treatment for 90min in an ice bath by using a 750W ultrasonic machine;
in S9, the lower precipitate after centrifugation was collected and 60mL of deionized water was added.
Example 4
Single-layer Ti 3 C 2 T X The colloid was prepared in substantially the same manner as in example 1, except that,
in S1, Ti is weighed respectively 3 AlC 2 2.000g (200mesh) of powder, 2.210g of anhydrous LiCl, and 30mL of a 37 wt% HCl solution.
Comparative example 1
Multilayer Ti 3 C 2 T X A method of preparing a powder comprising the steps of:
S1、separately weighing Ti 3 AlC 2 30mL of a HF solution (200mesh) containing 2.000g of powder and having a mass concentration of 40 wt%;
firstly, adding HF solution into a polytetrafluoroethylene bottle, and then adding Ti 3 AlC 2 Slowly adding the powder into the HF solution for 1min to obtain a solution A;
s2, placing the solution A on a magnetic stirrer to be stirred for 30min, placing the stirred mixed solution in an oven, and setting the temperature of the oven to be 60 ℃ to react for 24 h;
s3, cooling the reacted mixed solution in an oven to room temperature, taking out, adding 60mL of HCl solution (18% of mass fraction) into a plastic beaker, adding the cooled solution into the HCl solution, and standing for 4 hours or longer;
s4, pouring out the HCl solution on the upper layer when the reactant in the cup is precipitated to the bottom, and adding the precipitate on the bottom of the cup into four centrifuge tubes respectively for later use;
s5, adding deionized water into the centrifuge tube, centrifuging at 6000rpm for 10min, and pouring out supernatant;
s6, repeating the step S5 until the pH of the supernatant is 5, collecting the centrifuged lower precipitate, and placing the precipitate in a ventilated place to dry in natural air for 24-28 h to obtain the multilayer Ti 3 C 2 T X And (3) powder.
Multilayer Ti obtained as described above 3 C 2 T X An electron micrograph of the powder is shown in FIG. 5 (a).
Comparative example 2
Few layer of Ti 3 C 2 T X -a method for the preparation of Li powder comprising the following steps:
s1, respectively weighing Ti 3 AlC 2 2.000g (200mesh) of powder, 2.2112g of anhydrous LiCl and 30mL of a 40 wt% HF solution;
firstly, adding an HF solution into a polytetrafluoroethylene bottle, then adding anhydrous LiCl into the HF solution, and stirring and dissolving to obtain a solution A;
s2, slowly adding Ti into the solution A 3 AlC 2 Powder, the charging time is 1 min; after the feeding is finished,placing the reaction mixture on a magnetic stirrer, stirring for 30min, placing the stirred mixed solution in an oven, and setting the temperature of the oven to be 60 ℃ to react for 24 h;
s3, cooling the reacted mixed solution in an oven to room temperature, taking out, adding 60mL of HCl solution with the mass concentration of 18% into a plastic beaker, adding the cooled mixed solution into the HCl solution, and standing for 4 hours or longer;
s4, pouring out the HCl solution on the upper layer when the reactant in the cup is precipitated to the bottom, and adding the precipitate on the bottom of the cup into four centrifuge tubes respectively for later use;
s5, adding deionized water into the centrifuge tube, centrifuging at 6000rpm for 10min, and pouring out supernatant;
s6, repeating the step S5 until the pH value of the supernatant liquid is 5; collecting the centrifuged lower precipitate, and placing the precipitate in a ventilated place for drying in natural air for 24-28 h to obtain few-layer Ti 3 C 2 T X -Li powder. The above-obtained few-layer Ti 3 C 2 T X Electron microscopy images of the Li powder are shown in fig. 5(b) and (c).
The multilayer Ti obtained in comparative example 1 3 C 2 T X Powder, few-layer Ti obtained in comparative example 2 3 C 2 T X Li powder and Single-layer Ti obtained in example 1 3 C 2 T X The colloid was subjected to a small angle scattering experiment and the results are shown in fig. 6.
As can be seen from FIG. 6, the multilayer Ti of comparative example 1 3 C 2 T X Powder at 6nm -1 A diffraction peak appears at the position, and the few-layer Ti of comparative example 2 3 C 2 T X Li powder at 4.8nm -1 A diffraction peak appears at the position, both peaks correspond to the lamellar periodic structure, while the single-layer Ti of example 1 3 C 2 T X There is no diffraction peak, which indicates that Ti prepared in example 1 3 C 2 T X The colloid is in a monolithic layer structure. The monolithic layer Ti of example 1 was calculated by the Guinier's theorem of plate-like particles 3 C 2 T X The thickness of the lamella was 1.1 nm.
The multilayer Ti obtained in comparative example 1 3 C 2 T X Powder and Ti of less layer obtained in comparative example 2 3 C 2 T X Adsorption experiment of uranyl nitrate on Li powder, procedure of experiment and monolayer Ti obtained in example 1 3 C 2 T X The adsorption experiment process of uranyl nitrate carried out by the colloid is the same. Fig. 2 shows the adsorption performance results of the products obtained in example 1, comparative example 1, and comparative example 2 for uranyl u (vi). As can be seen from FIG. 2, the single-layer Ti obtained in example 1 3 C 2 T X The colloid has the best adsorption performance.
In summary, the results shown in FIGS. 2 and 3 show that the single-layer Ti obtained in example 1 3 C 2 T X The adsorption data of the colloid on uranyl are shown in Table 1 and FIG. 3, the maximum adsorption amount is 3.2mmol/g, and the colloid is the few-layer Ti of comparative example 2 3 C 2 T X Nearly 3 times the amount of adsorption of Li powder. From the above results, it can be seen that the single-layer Ti having high selective adsorption of uranyl group prepared in example 1 of the present invention 3 C 2 T X And (3) colloid.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The preparation method of the single-layer MXene colloid is characterized by comprising the following steps:
s1, dissolving anhydrous LiCl in inorganic acid to obtain a solution A; in S1, the inorganic acid is hydrofluoric acid and/or hydrochloric acid; the dosage ratio of LiCl to inorganic acid is 1 g: 10-20 mL;
s2, adding MXene precursor into the solution A, and reacting at 50-60 ℃; in S2, the mass ratio of MXene precursor to LiCl is 1: 1-2;
s3, adding the reaction solution of S2 into a hydrochloric acid solution, and then standing for reaction; after the reaction is finished, repeatedly adding water into the lower-layer precipitate for centrifugation until the pH value of the upper-layer clarified liquid is 5;
s4, adding ethanol into the lower-layer precipitate of the S3, and carrying out ultrasonic treatment and separation; then collecting the lower-layer precipitate, adding water, performing ultrasonic treatment and separation, and collecting the upper-layer liquid to obtain a single-layer MXene colloid.
2. The method of claim 1, wherein the MXene precursor in S2 is Ti 3 AlC 2 、Ti 2 AlC、V 2 AlC、Nb 2 Any one or a mixture of more of AlC.
3. The method for preparing the single-layer MXene colloid according to claim 1, wherein in S3, the dosage ratio of MXene precursor to hydrochloric acid solution is 1 g: 30 mL; the mass concentration of the hydrochloric acid solution is 18%.
4. The method for preparing the single-layer MXene colloid according to claim 1, wherein in S4, the solution before ultrasonic treatment needs to be treated with nitrogen for 20 min; the ultrasonic process is carried out in an ice bath at 0-4 ℃; the ultrasonic time is 20-90 min.
5. The method for preparing the single-layer MXene colloid according to claim 1, wherein the ratio of MXene precursor to water in S4 is 1 g: 20-60 mL.
6. A monolayer MXene colloid prepared by the method of claim 1.
7. Use of the monolayer MXene colloid of claim 6 for selective adsorption removal of uranyl ions.
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