CN114160091A - Preparation method of hydroxyl functionalized titanium carbide and application of hydroxyl functionalized titanium carbide in efficient adsorption and cesium removal - Google Patents
Preparation method of hydroxyl functionalized titanium carbide and application of hydroxyl functionalized titanium carbide in efficient adsorption and cesium removal Download PDFInfo
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- CN114160091A CN114160091A CN202111462919.9A CN202111462919A CN114160091A CN 114160091 A CN114160091 A CN 114160091A CN 202111462919 A CN202111462919 A CN 202111462919A CN 114160091 A CN114160091 A CN 114160091A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses a preparation method of hydroxyl functionalized titanium carbide and application of the hydroxyl functionalized titanium carbide in efficient adsorption and cesium removal, belongs to the field of radionuclide sewage treatment, and aims to solve the problem of low cesium removal adsorption rate of the existing adsorbent. The preparation method comprises the following steps: firstly, dispersing titanium aluminum carbide in a hydrofluoric acid solution to prepare titanium carbide precursor powder, dispersing the titanium carbide precursor powder in a DMSO solution, stirring, and then carrying out ultrasonic treatment to obtain a titanium carbide material; and secondly, dispersing the titanium carbide material in a potassium hydroxide solution, stirring at room temperature, washing the solid phase with water, centrifuging and drying to obtain the hydroxyl functionalized titanium carbide. The invention discovers that the hydroxyl functionalized titanium carbide is used for preparing Cs+The titanium carbide is subjected to surface modification by potassium hydroxide, and the preparation condition and the adsorption condition of the adsorbent are optimized to ensure that the Cs has high adsorption rate+The adsorption rate of (A) was increased from 50% to about 90%. The high-efficiency cesium removal adsorbent Ti3C2The preparation process of OH is simple, and the adsorption condition is mild and controllable.
Description
Technical Field
The invention belongs to the field of radionuclide sewage treatment, and particularly relates to a preparation method of hydroxyl functionalized titanium carbide and application thereof in efficient adsorption and cesium removal.
Background
Radioactive cesium (137Cs) is one of the most dangerous elements of radionuclides, has a high fission yield (6.09%), a long half-life (30.2 years), high energy gamma radiation, and high solubility and volatility in water. Due to Cs+Has a reaction with K+、Na+Similar biological properties, can enter the human body, causing serious health problems. Therefore, to solve these problems, low-radioactive Cs are effectively removed+Nuclear waste water of (a) is urgently needed. In recent years, for Cs in aqueous solution+The removing method mainly comprises a solvent extraction method, an adsorption method, a chemical precipitation evaporation method, a membrane technology and the like. Large scale application of solvent extraction is limited due to high chemical and equipment costs. The evaporation method also has disadvantages such as corrosion, fouling or foaming. Wherein the adsorption method is an efficient, simple, economical and convenient method. It remains a challenge to select an adsorbent with high selectivity, high adsorption rate and low cost. At present, reported on Cs+The adsorbent with adsorption effect includes titanate, vanadate, tungsten-based material, manganese oxide, ferrite hexacyanate, metal sulfide, molybdenum ammonium phosphate, hydroxyapatite, etc. Titanium carbide (Ti)3C2) The titanium carbide is a new two-dimensional nano material produced by stripping or etching, and has the advantages of good chemical stability, adjustable chemical properties, high hydrophilicity, excellent ion intercalation capability and strong negative charges on the surface. Titanium carbide has a larger specific surface area and more functional groups per unit mass due to its layered structure than other two-dimensional materials, and thus has a higher affinity for Cs in aqueous solution+Has larger adsorption capacity. Titanium carbide to Cs+The adsorption mechanism is as follows:
Ti3C2(s)+H2O(l)→Ti3C2OH(s)+1/2H2(g) (1)
Ti3C2(s)+HF(aq)→Ti3C2F(s)+1/2H2(g) (2)
[Ti-O]-H+→Ti-OCs (3)
however, the maximum adsorption rate is only 50%, and therefore, it is necessary to further increase the cesium removal adsorption rate of titanium carbide.
Disclosure of Invention
The invention aims to solve the problem of low cesium removal adsorption rate of the existing adsorbent, and provides a preparation method of hydroxyl functionalized titanium carbide and application of the hydroxyl functionalized titanium carbide in high-efficiency cesium removal adsorption.
The preparation method of the hydroxyl functionalized titanium carbide is realized according to the following steps:
firstly, dispersing titanium aluminum carbide in a hydrofluoric acid solution, stirring the obtained suspension at room temperature, then centrifuging, filtering, washing and drying to obtain titanium carbide precursor powder, dispersing the titanium carbide precursor powder in a DMSO solution, stirring for 22-25 h, then performing ultrasonic treatment, centrifuging, washing and drying to obtain a titanium carbide material;
secondly, mixing titanium carbide (Ti)3C2) Dispersing the material in potassium hydroxide (KOH) solution, stirring at room temperature, washing the solid phase with water, centrifuging, and drying to obtain hydroxyl-functionalized titanium carbide (Ti)3C2OH)。
The application of the hydroxyl functional titanium carbide of the invention is that the hydroxyl functional titanium carbide is added to the Cs-containing material as an adsorbent+The water of (3) is cesium-removed.
In the first step of the invention, hydrofluoric acid is selected to selectively etch aluminum in titanium aluminum carbide, the titanium carbide material product contains F element, and then potassium hydroxide is used for hydroxylation, so that the F element is more easily replaced by hydroxyl.
The invention provides a preparation method of hydroxyl functionalized titanium carbide of an efficient cesium removal adsorbent, which comprises the following steps: namely, hydroxyl in potassium hydroxide is modified on a two-dimensional material titanium carbide by adopting a one-step method to obtain the high-efficiency cesium-removing adsorbent Ti3C2OH, the adsorbent can realize 90% of cesium removal efficiency after simple hydroxyl functionalization by optimizing the preparation condition and the adsorption condition of the adsorbent.
The preparation method and the application of the hydroxyl functionalized titanium carbide comprise the following beneficial effects:
the invention discovers that the hydroxyl functionalized titanium carbide is used for Cs for the first time+High adsorption rate, surface modification of titanium carbide by potassium hydroxide, andoptimizing the preparation condition and adsorption condition of the adsorbent to ensure that the Cs+The adsorption rate of (A) was increased from 50% to about 90%. The high-efficiency cesium removal adsorbent Ti3C2The preparation process of OH is simple, the adsorption condition is mild and controllable, only potassium hydroxide solution is needed, the cost is reduced, and the excellent cesium removal rate of 90% is realized.
Drawings
FIG. 1 shows Ti in example3C2XRD pattern of OH material, wherein 5 represents Ti3AlC2Material, 4 represents Ti3C2Material, 3 represents 8 wt.% Ti3C2OH material (example three), 2 represents 10 wt.% Ti3C2OH (example one), 1 represents 12 wt.% Ti3C2OH (example two);
FIG. 2 is an XRD pattern with the abscissa of 4-12 in FIG. 1, wherein 5 represents Ti3AlC2Material, 4 represents Ti3C2Material, 3 represents 8 wt.% Ti3C2OH material (example three), 2 represents 10 wt.% Ti3C2OH (example one), 1 represents 12 wt.% Ti3C2OH (example two);
FIG. 3 shows the application of Ti in the examples3C2The cesium removal rate of OH material is measured, wherein ■ represents Ti3C2Material, a represents 8 wt.% Ti3C2OH Material (example III), ● represents 10 wt.% Ti3C2OH (example one), t.t. represents 12 wt.% Ti3C2OH (example two).
Detailed Description
The first embodiment is as follows: the preparation method of the hydroxyl-functionalized titanium carbide of the embodiment is implemented as follows:
firstly, dispersing titanium aluminum carbide in a hydrofluoric acid solution, stirring the obtained suspension at room temperature, then centrifuging, filtering, washing and drying to obtain titanium carbide precursor powder, dispersing the titanium carbide precursor powder in a DMSO solution, stirring for 22-25 h, then performing ultrasonic treatment, centrifuging, washing and drying to obtain a titanium carbide material;
secondly, mixing titanium carbide (Ti)3C2) Dispersing the material in potassium hydroxide (KOH) solution, stirring at room temperature, washing the solid phase with water, centrifuging, and drying to obtain hydroxyl-functionalized titanium carbide (Ti)3C2OH)。
In the first step of the embodiment, aluminum titanium carbide and hydrofluoric acid solution are used as raw materials, aluminum in the aluminum titanium carbide is selectively etched by the hydrofluoric acid solution to synthesize a titanium carbide base material, and then the titanium carbide is subjected to functional modification, namely, the titanium carbide is subjected to hydroxylation modification by using potassium hydroxide as a hydroxyl source and adopting a one-step surface modification method to prepare Ti3C2An OH material.
According to the embodiment, the hydroxyl functionalized titanium carbide material is used for removing cesium in water, so that the cesium removal efficiency is improved.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the suspension in the first step is stirred for 46-50 hours at room temperature.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the drying in the first step is drying for 8-10 h at 60 ℃ in air atmosphere.
The fourth concrete implementation mode: the present embodiment is different from one of the first to third embodiments in that the time for the ultrasonic treatment in the first step is 1 h.
The fifth concrete implementation mode: the difference between the first embodiment and the fourth embodiment is that the mass ratio of the titanium aluminum carbide to the hydrofluoric acid in the first step is 1: 22.4-1: 23.6.
The sixth specific implementation mode: the difference between the embodiment and one of the first to fifth embodiments is that the molar ratio of the titanium aluminum carbide to the DMSO in the first step is 1: 20.4-1: 28.6.
The seventh embodiment: the difference between the present embodiment and one of the first to sixth embodiments is that the mass fraction of the potassium hydroxide solution in the second step is 8% to 12%.
The specific implementation mode is eight: the difference between the present embodiment and one of the first to seventh embodiments is that the stirring time at room temperature in the second step is 4 to 5 hours.
The specific implementation method nine: this embodiment hydroxyl functionalizationThe application of the titanium carbide is that hydroxyl functionalized titanium carbide is added to Cs-containing substances as an adsorbent+The water of (3) is cesium-removed.
The detailed implementation mode is ten: the present embodiment differs from the ninth embodiment in that the pH of the adjustment system is 5 to 9.
The first embodiment is as follows: the preparation of hydroxyl-functionalized titanium carbide according to this example was carried out as follows:
firstly, dispersing 2.0g of titanium aluminum carbide in 40mL of hydrofluoric acid solution, stirring the obtained suspension for 48h at room temperature, centrifuging, filtering, washing with water and ethanol for 3 times respectively, drying at 60 ℃ in the air atmosphere for 8h to obtain titanium carbide precursor powder, dispersing the titanium carbide precursor powder in 30mL of DMSO solution, stirring for 24h, then performing ultrasonic treatment for 1h, centrifuging, washing and drying to obtain a titanium carbide material;
secondly, 0.1g of titanium carbide (Ti)3C2) The material was dispersed in 5mL of 10 wt.% potassium hydroxide (KOH) solution, stirred at room temperature for 4h, and the solid phase was washed with water, centrifuged (until pH 6), and dried to obtain hydroxyl-functionalized titanium carbide.
Ti obtained in example3C2XRD patterns of OH materials are shown in FIGS. 1 and 2, with FIG. 1 showing Ti3C2OH still has the characteristic peak of titanium carbide, the hydroxyl functional modification of potassium hydroxide does not change the structure of the titanium carbide material, and the hydroxyl number in the titanium carbide material is increased through the treatment of potassium hydroxide, as shown in figure 3, the content of the hydroxyl in the aqueous solution to Cs is greatly improved+The adsorption rate of (3).
Example two: the difference between this example and the first example is that in the second step, 0.1g of titanium carbide is dispersed in 5mL of 12 wt.% potassium hydroxide solution, stirred at room temperature for 4h, and the solid phase is washed with water, centrifuged (until pH 6), and dried to obtain hydroxyl-functionalized titanium carbide.
Example three: the difference between this example and the first example is that in the second step, 0.1g of titanium carbide is dispersed in 5mL of 8 wt.% potassium hydroxide solution, stirred at room temperature for 4h, and the solid phase is washed with water, centrifuged (until pH 6), and dried to obtain hydroxyl-functionalized titanium carbide.
From the cesium removal rate plot of FIG. 2, 10 wt.% Ti was found in all samples3C2The cesium removal rate of OH reaches the highest. The sample has more hydroxyl groups and the highest cesium removal rate, so that more ideal adsorption activity is obtained.
The first application embodiment: in this example, 0.05g of pure titanium carbide was placed in 50mL of cesium chloride solution, Cs+The concentration of (2) was 5mg/L, and the pH of the system was adjusted to 7 with a dilute hydrochloric acid solution, and magnetic stirring adsorption was performed to balance the adsorption.
In this example, an adsorbent in the reaction solution was removed by a water filter (0.22 μm), and Cs remaining in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp+And (4) concentration. The cesium removal rates were measured at 6.55%, 22.5%, 33.1%, 41.5%, and 47.3% for each of the reaction time intervals of 1min, 5min, 10min, 30min, and 60 min.
Application example two: this example 0.05g of the hydroxy-functionalized titanium carbide obtained in example one was placed in 50mL of cesium chloride solution, Cs+The concentration of (3) was 5mg/L, and the pH of the system was 7, and magnetic stirring adsorption was performed to make the adsorption balanced.
In this example, an adsorbent in the reaction solution was removed by a water filter (0.22 μm), and Cs remaining in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp+And (4) concentration. The cesium removal rates were measured at 1min, 5min, 10min, 30min, and 60min reaction time intervals, respectively, as 82.4%, 85.5%, 86.1%, 86.3%, and 86.3%.
Application example three: in this example, 0.05g of the hydroxy-functionalized titanium carbide obtained in example III was placed in 50mL of cesium chloride solution, Cs+The concentration of (3) was 5mg/L, and the pH of the system was 7, and magnetic stirring adsorption was performed to make the adsorption balanced.
In this example, an adsorbent in the reaction solution was removed by a water filter (0.22 μm), and Cs remaining in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp+And (4) concentration. The cesium removal rates were measured at 49.9%, 66.7%, 69.4%, 75.3%, 76.7% in each of the reaction time intervals of 1min, 5min, 10min, 30min, 60 min.
Application example four: in this example, 0.05g of the hydroxy-functionalized titanium carbide obtained in example two was placed in 50mL of cesium chloride solution, Cs+The concentration of (3) was 5mg/L, and the pH of the system was 7, and magnetic stirring adsorption was performed to make the adsorption balanced.
In this example, an adsorbent in the reaction solution was removed by a water filter (0.22 μm), and Cs remaining in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp+And (4) concentration. The cesium removal rates were measured at reaction time intervals of 1min, 5min, 10min, 30min, and 60min, respectively, to be 47.0%, 61.4%, 64.8%, 70.1%, and 73.5%.
Application example five: in this example, 0.05g of the hydroxyl-functionalized titanium carbide obtained in the first example was placed in 50mL of a cesium chloride solution, the Cs + concentration was 5mg/L, the pH of the system was adjusted to 5 with a dilute hydrochloric acid solution, and magnetic stirring adsorption was performed to equilibrate the adsorption.
In this example, the adsorbent in the reaction solution was removed by a water system filter head (0.22 μm), and the remaining Cs + concentration in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp. The cesium removal rates were measured at 64.7%, 78.2%, 84.4%, 85.7%, 85.9% in each of the reaction time intervals of 1min, 5min, 10min, 30min, and 60 min.
Application example six: in this example, 0.05g of the hydroxyl-functionalized titanium carbide obtained in the first example was placed in 50mL of a cesium chloride solution, the Cs + concentration was 5mg/L, the pH of the system was adjusted to 9 with a dilute potassium hydroxide solution, and magnetic stirring adsorption was performed to equilibrate the adsorption.
In this example, an adsorbent in the reaction solution was removed by a water filter (0.22 μm), and Cs remaining in the solution was measured by an atomic absorption spectrometer using a Cs hollow cathode lamp+And (4) concentration. The cesium removal rates were measured at 38.7%, 40.1%, 44.0%, 47.6%, 58.0% in each of the reaction time intervals of 1min, 5min, 10min, 30min, 60 min.
Claims (10)
1. The preparation method of the hydroxyl functionalized titanium carbide is characterized by comprising the following steps:
firstly, dispersing titanium aluminum carbide in a hydrofluoric acid solution, stirring the obtained suspension at room temperature, then centrifuging, filtering, washing and drying to obtain titanium carbide precursor powder, dispersing the titanium carbide precursor powder in a DMSO solution, stirring for 22-25 h, then performing ultrasonic treatment, centrifuging, washing and drying to obtain a titanium carbide material;
and secondly, dispersing the titanium carbide material in a potassium hydroxide solution, stirring at room temperature, washing the solid phase with water, centrifuging and drying to obtain the hydroxyl functionalized titanium carbide.
2. The method according to claim 1, wherein the suspension is stirred at room temperature for 46-50 h.
3. The method according to claim 1, wherein the drying in the first step is performed at 60 ℃ for 8 to 10 hours in an air atmosphere.
4. The method according to claim 1, wherein the time for the ultrasonic treatment in the first step is 1 hour.
5. The method for preparing hydroxyl-functionalized titanium carbide according to claim 1, wherein the mass ratio of the titanium aluminum carbide to the hydrofluoric acid in the first step is 1: 22.4-1: 23.6.
6. The method for preparing hydroxyl-functionalized titanium carbide according to claim 1, wherein the molar ratio of the titanium aluminum carbide to the DMSO in the first step is 1: 20.4-1: 28.6.
7. The method for preparing hydroxyl-functionalized titanium carbide according to claim 1, wherein the mass fraction of the potassium hydroxide solution in the second step is 8-12%.
8. The method for preparing hydroxyl-functionalized titanium carbide according to claim 1, wherein the stirring time in the second step at room temperature is 4-5 h.
9. The use of hydroxyl-functionalized titanium carbide according to claim 1 wherein the hydroxyl-functionalized titanium carbide is added as an adsorbent to the Cs-containing material+The water of (3) is cesium-removed.
10. The use of hydroxyl-functionalized titanium carbide according to claim 9, wherein the pH of the adjustment system is 5 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115845815A (en) * | 2022-11-17 | 2023-03-28 | 赣南科技学院 | Preparation method of Fe @ C/MXene-APTS magnetic composite material |
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| CN106268610A (en) * | 2016-10-11 | 2017-01-04 | 东南大学 | A kind of preparation method of two dimension titanium carbide adsorbing material |
| CN109569495A (en) * | 2019-01-18 | 2019-04-05 | 广西大学 | High-specific surface area carbonization titanium material and preparation method thereof |
| CN113003675A (en) * | 2021-02-05 | 2021-06-22 | 南方科技大学 | Mxene material with organic chelating functional group grafted on surface and preparation method thereof |
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| CN105304154A (en) * | 2014-07-03 | 2016-02-03 | 中国科学院宁波材料技术与工程研究所 | Application of two-dimensional transitional metal carbide nanosheet as radionuclide adsorbent |
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| CN109569495A (en) * | 2019-01-18 | 2019-04-05 | 广西大学 | High-specific surface area carbonization titanium material and preparation method thereof |
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