Carboxyaryl functionalized MXene material as well as preparation method and application thereof
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A technology of carboxyl functionalization and functionalization, which is applied in the field of two-dimensional materials, can solve safety problems and other problems, and achieve the effects of less pollution, improved binding ability and complexation ability with heavy metals, and easy separation
Active Publication Date: 2020-06-05
HUAIYIN TEACHERS COLLEGE
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However, the raw material hydrogen peroxide is regulated due to safety issues
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Embodiment 1
[0058] Example 1Ti 3 C 2 preparation of
[0059] (1) Etching Ti 3 AlC 2 :
[0060] After dissolving LiF (2.6g) in 30ml of 12mol / L hydrochloric acid solution and 9ml of water at room temperature, the solution was heated to 40°C and continued to stir for 10min; 3 AlC 2 (2g) Add a small amount to the above solution in batches, continue to stir at 40°C for 27h, completely remove the Al element in the compound, and obtain an accordion-shaped compound with Ti 3 C 2 The multi-layer MXene material of the structural formula, the mixture is subjected to centrifugation, washing, ultrasonication, and vacuum drying to obtain Ti 3 C 2 T m (MXene material), T m Is the surface group F, Cl or OH.
[0061] (2) 1.0g Ti obtained in step 1 3 C 2 T m Add it to 20ml of 4mol / L KOH solution, stir at room temperature for 7h, centrifuge to obtain a solid precipitate, wash the solid with water until the eluate is neutral, and then disperse the solid in 10ml of water to obtain a suspension...
Embodiment 2
[0071] Example 2 Ti 3 C 2 Preparation of supported palladium catalyst
[0072] 200mg of Ti prepared 3 C 2 Add 5ml of water and 15ml of methanol, stir at 30°C for 30min, then add NaPdCl to the mixture 4 (0.01g), after stirring for 1h, it was placed in a hydrothermal kettle and aged at 120°C for 16h, finally centrifuged, washed with water and alcohol for several times, and then vacuum-dried for 10h to obtain the catalyst Ti 3 C 2 supported palladium catalyst.
[0073] The Pd loading was 1.80 wt%. Through the nitrogen adsorption-desorption isotherm test, it was found that the specific surface area decreased, which proved that the Pd catalyst was successfully loaded, and the actual loading amount of the ICP-MS test was 1.75wt%.
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Abstract
The invention discloses a carboxyaryl functionalized MXene material. The carboxyaryl functionalized MXene material has a Mn+1Xn-Ph(COOH)2 structure, wherein M is any one or at least two metal elementsin the IIIB group, the IVB group, the VB group, the VIB group and the VIIB group; X is any one or a combination of two of C and N elements; and n is 1, 2 or 3. The carboxyaryl functionalized MXene material has strong complexing ability with heavy metals, and can catalyze the reaction of synthesizing phenol from arylboronic acid, thereby avoiding the use of hydrogen peroxide and enhancing the safety of the synthesis method. The invention also discloses a preparation method of the carboxyaryl functionalized MXene material, which comprises the following steps: carrying out alkaline hydrolysis onthe MXene material, and carrying out a diazotization reaction on the hydrolyzed MXene material and aminobenzenedicarboxylic acid to obtain the carboxyaryl functionalized MXene new material. The preparation process is simple, feasible and mild in condition. The invention also discloses an application of the carboxyaryl functionalized MXene material in wastewater purification and catalysis of in-situ hydroxylation of arylboronic acid to synthesize phenol. The invention also discloses a carboxyaryl functionalized MXene material supported palladium catalyst as well as a preparation method and anapplication thereof.
Description
technical field [0001] The invention relates to the technical field of two-dimensional materials, in particular to a carboxyl-functionalized MXene material and its preparation method and application. Background technique [0002] MXene materials are a class of layered two-dimensional carbon / nitrides, which are usually extracted from their parent phase material MAX phase (M n+1 AX n , n=1-3, M is a transition metal, A is a IIIA or IVA group element, and x is C or N) in A layer atomic layer. Due to its high specific surface area, hydrophilicity, adsorption and high surface reactivity, MXene has attracted extensive attention from researchers in many fields, and can be used in many fields such as adsorption of heavy metals, supercapacitors, lithium-ion batteries, catalysis, etc. . [0003] The surface of MXene prepared by etching the MAX phase with an acidic solution containing fluoride often contains groups such as -OH, -Cl and -F, abbreviated as M n+1 x n T m , where T ...
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