Preparation and application of mercapto modified metal-organic frameworks catalyst

A metal-organic framework and sulfhydryl modification technology, which can be used in the preparation of organic compounds, the preparation of carbon-based compounds, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problems affecting the photocatalytic performance of noble metal/MOF composites. , to achieve good benzaldehyde selectivity, good catalytic activity, and the effect of improving light absorption performance

Active Publication Date: 2017-10-10
FUZHOU UNIV
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  • Claims
  • Application Information

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Problems solved by technology

The above methods generally require supporting chemical reactors or harsh reaction conditions. The reducing agent sodium borohydride used in the chemical reduction method will largely destroy the structure of MOFs materials. In addition, PVP is often added during the synthesis process. Such as organic macromolecular polymers to control the size of noble metal particles and prevent the agglomeration of noble metals, but it is difficult to completely remove PVP after noble metal loading, which greatly affects the photocatalytic performance of noble metal / MOF composites

Method used

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  • Preparation and application of mercapto modified metal-organic frameworks catalyst
  • Preparation and application of mercapto modified metal-organic frameworks catalyst
  • Preparation and application of mercapto modified metal-organic frameworks catalyst

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Experimental program
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Effect test

Embodiment 1

[0029] UiO-66(SH) 2 Specific preparation of photocatalyst

[0030] Weigh zirconium tetrachloride and 2,5-dimercapto-1,4-terephthalic acid with a molar ratio of 1:1, dissolve them in 50 mL DMF, stir at room temperature until the solution is homogeneous and transparent, then transfer to a 100 mL high-pressure In the reactor, it was kept at 120 °C for 24 h. After the obtained sample was cooled naturally, it was heated and stirred with DMF at 60 °C for 2 h, and then the residual DMF was exchanged with dichloromethane, and the yellow powder UiO-66(SH) was obtained after vacuum drying at 100 °C for 12 h. 2 . figure 1 Demonstrate the UiO-66(SH) prepared by this method 2 XRD pattern with UiO-66, it can be seen that UiO-66(SH) 2 Has the same topology as UiO-66. figure 2 Demonstrated UiO-66(SH) 2 Compared with the DRS diagram of UiO-66, the modification of sulfhydryl group can successfully broaden the absorption band edge of UiO-66 from the ultraviolet region (320 nm) to the visi...

Embodiment 2

[0032] M / UiO-66(SH) 2 Preparation of (M=Au, Pd, Pt) Composite Photocatalytic Materials

[0033] First take by weighing the UiO-66 (SH) that embodiment 1 makes 2 100 mg of sample was ultrasonically dispersed in 40 mL of ethanol and water (v: v = 1:1) solution, and a certain volume of metal precursor (0.420 ml HAuCl 4 , 0.332 ml H 2 PdCl 4 or 0.530 ml H 2 PtCl 6 (both 10 mg / mL)) solution was added dropwise to the mixed solution. After stirring for 12 h, the obtained sample is M / UiO-66(SH) 2 (M=Au, Pd, Pt). Figure 4 Demonstrated UiO-66(SH) 2 and M / UiO-66(SH) 2 The XRD pattern. Figure 5 Showcasing the M / UiO-66(SH) 2 It can be seen from the figure that the presence of metal particles was not observed in high-resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM), but the uniform distribution of noble metals was detected in the selected element scanning. Explain the preparation of M / UiO-66(SH) by using mercapto-anch...

Embodiment 3

[0035] UiO-66(SH) 2 Activity of Photocatalytic Selective Oxidation of Benzyl Alcohol at Room Temperature

[0036] Weigh 20 mg of the prepared catalyst sample with an analytical balance, and pipette 1.5 mL and 0.1 mmol of the reaction substrate in trifluorotoluene solution filled with saturated air and nitrogen respectively with a pipette gun, and place them together in a Pyrex glass tube. Connect a balloon filled with the corresponding gas at a pressure of 0.1 MPa to ensure the gas atmosphere. After ultrasonic dispersion, the sample was irradiated with xenon lamp to simulate visible light (λ ≥ 420 nm) for 12 h, then centrifuged and the chemical components in the supernatant were detected by gas chromatography. The results are shown in Table 1, the overall conversion rate under nitrogen atmosphere is higher than that under atmospheric atmosphere. It can be seen from Nos. 2 and 3 that when there is –CH at the para-position of the benzene ring 3 and –OCH 3 When the power s...

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Abstract

The invention discloses preparation methods and application of a mercapto MOFs (Metal-Organic Frameworks) photocatalyst UiO-66(SH)2 and a series of noble metal mercapto MOFs photocatalysts M/UiO-66(SH)2 (M=Au, Pd and Pt). The UiO-66(SH)2 is prepared based on a pre-functionalization strategy by using zirconium tetrachloride and 2,5-dimercapto-1,4-terephthalic acid as precursors and combining with a solvent thermal synthesis method. By utilizing the metal affine effect of a mercapto functional group on a ligand skeleton, a noble metal ion is anchored on the UiO-66(SH)2, so that an M/UiO-66(SH)2 composite photocatalytic material is successfully prepared. In a loading process, an inert atmosphere, the addition of a strong reducing agent or a heat treatment process is not needed; highly dispersed Au, Pd and Pt ions can be loaded on a UiO-66(SH)2 material through a simple mixing process only. The UiO-66(SH)2 and the M/UiO-66(SH)2 both show favorable activity in an experiment of photocatalytically selectively oxidizing benzyl alcohol.

Description

technical field [0001] The invention belongs to the field of photocatalysis and organic synthesis, in particular to UiO-66(SH) 2 And its derived series precious metal M / UiO-66(SH) 2 (M=Au, Pd, Pt) catalysts, including their preparation and applications. Background technique [0002] Metal-organic frameworks (MOFs) are three-dimensional porous materials with periodic network structures formed by self-assembly of organic ligands and metal ions. It has the advantages of large specific surface area, strong designability and easy modulation. The metal-oxygen clusters of many MOFs materials have semiconductor-like properties, combined with the tailorability and modification of their own channels, as well as the functionality endowed by the metal center, unsaturated metal sites and dynamic framework structures, etc., so MOFs materials can be combined With the dual properties of semiconductor and molecular sieve, it can be used in photolysis of water, CO 2 It shows its applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C45/00C07C47/54C07C47/542C07C47/575C07C47/55C07C47/02C07C201/12C07C205/44C07B41/06
CPCB01J31/1691B01J31/2247B01J31/226B01J35/004B01J2231/763B01J2531/48C07B41/06C07C45/002C07C201/12C07C47/54C07C47/542C07C47/575C07C47/55C07C47/02C07C205/44
Inventor 吴棱陈蕊王志同荆凯强申川
Owner FUZHOU UNIV
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