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Rare earth metal complex, preparation method thereof and photocatalyst

A technology of rare earth metals and photocatalysts, applied in the field of photocatalysis, can solve the problems of limiting the catalytic activity of catalysts, and achieve the effects of excellent photocatalytic cracking water hydrogen production activity and stability, easy availability of raw materials, and simple synthesis methods

Pending Publication Date: 2022-07-22
BEIJING BUILDING MATERIALS ACADEMY OF SCI RES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For most photocatalysts, there is a problem of rapid recombination of photogenerated electron-holes, which limits the catalytic activity of the catalysts.
Moreover, there is still room for improvement in the application effect of rare earth metal complexes of diphenylphosphonic acid in photocatalytic hydrogen production in existing studies. At present, a new type of rare earth metal complexes for photocatalytic cracking of water to produce hydrogen is designed and synthesized. Important issues to be solved in this field

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  • Rare earth metal complex, preparation method thereof and photocatalyst
  • Rare earth metal complex, preparation method thereof and photocatalyst
  • Rare earth metal complex, preparation method thereof and photocatalyst

Examples

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Embodiment 1

[0036] This embodiment provides rare earth metal complexes, figure 1 Shown is the synthesis reaction equation of the rare earth metal complex. Specifically, the synthesis method of the rare earth metal complex provided in this embodiment includes the following steps:

[0037] (1) Samarium chloride hexahydrate SmCl 3 ·6H 2 O (0.1824 g, 0.5 mmol), phenylphosphonic acid PPA (0.1186 g, 0.75 mmol) were dissolved in 7 mL of absolute ethanol, and the mixture was stirred at room temperature for 20 min until homogeneous.

[0038](2) The mixture was transferred to a 15 mL polytetrafluoroethylene-lined stainless steel autoclave, and the autoclave was placed in a muffle furnace. The reaction kettle was kept at a constant temperature of 180°C for 72h.

[0039] (3) after the reaction time finishes, take out the autoclave, naturally cool to room temperature, open the reactor, filter, wash with absolute ethanol, and dry in air to obtain a white sample (samarium phenylphosphonate complex), ...

Embodiment 2

[0045] This example provides the characterization of the rare earth metal complex in Example 1

[0046] Firstly, the morphology of MPPA (M=Sm, Y, Tb) was analyzed by scanning electron microscope (SEM). like figure 2 As shown, the morphologies of the complexes are all sheet-like, and the lengths of SmPPA, YPPA and TbPPA range from 1 μm to 6 μm, 0.5 μm to 3 μm and 0.5 μm to 2 μm, respectively, and the surface is smooth and uniformly distributed.

[0047] MPPA (M=Sm, Y, Tb) was determined by X-ray diffraction (XRD) ( image 3 ). It can be seen from the figure that the complexes are all crystalline compounds, and there are strong diffraction peaks at 2θ=5.68°, 5.74° and 5.80°, respectively, which belong to the characteristic diffraction peaks of samarium phenylphosphonate, iridium and terbium, respectively. .

[0048] In order to further determine the chemical composition of the complex MPPA (M=Sm, Y, Tb), its infrared absorption spectrum was measured ( Figure 4 ). Taking ...

Embodiment 3

[0051] This example provides the thermal behavior analysis of the rare earth metal complex in Example 1

[0052] The thermal behavior of MPPA (M=Sm, Y, Tb) was analyzed by thermogravimetry. Taking SmPPA as an example, there are three obvious weight loss intervals on the TG curve of SmPPA ( Image 6 ). The maximum weight loss temperatures of SmPPA in the three weight loss intervals were 128.9°C, 191.3°C and 617.1°C, and the weight loss rates were 2.16%, 2.20% and 18.20%, respectively. When the temperature was 800°C, the total weight loss and residual amount of the complex were 22.56% and 77.44%, respectively. It can be seen that SmPPA in N 2 Excellent thermal stability under atmosphere.

[0053] The changing trends of the thermogravimetric curves of YPPA and TbPPA are basically the same as those of SmPPA, and there are three obvious weight loss intervals on the TG curves ( Figure 7-8 ). Among them, the maximum weight loss temperature and weight loss of YPPA and TbPPA in ...

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Abstract

The invention relates to the field of photocatalysis, in particular to a rare earth metal complex, a preparation method thereof and a photocatalyst. The preparation method of the rare earth metal complex comprises the following steps: dissolving rare earth metal salt and phenylphosphonic acid in a solvent for solvothermal reaction to obtain the complex; wherein the rare earth metal salt is selected from at least one of samarium chloride hexahydrate, iridium chloride hexahydrate and terbium chloride hexahydrate; the molar ratio of the rare earth metal salt to the phenylphosphonic acid is 1: (0.5-8). The solvothermal synthesis method adopted by the invention is simple, the reaction condition is mild, and the novel phenylphosphonic acid rare earth metal complex prepared from the specific rare earth metal salt and phenylphosphonic acid has more excellent photocatalytic water splitting hydrogen production activity and stability.

Description

technical field [0001] The invention relates to the technical field of photocatalysis, in particular to a rare earth metal complex, a preparation method thereof, and a photocatalyst. Background technique [0002] Inorganic-organic hybrid materials are widely used in optical materials, biological materials, luminescent materials, catalysts, etc. due to the combination of the comprehensive properties of inorganic and organic components. There are many kinds of organic ligands, and phosphonic acids and carboxylic acids are common organic ligands. Compared with most carboxylic acid ligands, phosphonic acid ligands can form stronger coordination bonds with coordinating central ions. During the coordination process, the phosphonic acid ligands can provide different levels of deprotonation and more bonding sites, so the phosphonic acid complexes can exhibit better chemical and thermal stability. For example, the platinum(II) complexes synthesized by Zhang's group using 1,3-propan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/00C01B3/04C07F9/38
CPCC07F9/3834B01J31/1865C01B3/042B01J2531/38B01J35/39
Inventor 李爱红毛建伟杨楠李寅明郭建平
Owner BEIJING BUILDING MATERIALS ACADEMY OF SCI RES