Bismuth-based metal organic framework material as well as preparation method and application thereof
An organic framework and metal-based technology, applied in organic chemical methods, bismuth organic compounds, organic chemistry, etc., can solve the problems of poor electronic conductivity and unfavorable electron transfer of related MOFs, and achieve good photocatalytic reduction performance, low cost, The effect of high yield
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[0031] In yet another specific embodiment of the present invention, the preparation method includes: adding triphenylbismuth and 4-mercaptobenzoic acid into an organic solvent, adding benzoic acid at the same time, mixing evenly, and heating to reflux to obtain the product. In the preparation method, using triphenylbismuth as the Bi source can effectively avoid the hydrolysis of Bi.
[0032] In yet another specific embodiment of the present invention, the organic solvent includes xylene, toluene, carbon tetrachloride, etc., preferably xylene;
[0033] In yet another specific embodiment of the present invention, the molar ratio of the triphenylbismuth, 4-mercaptobenzoic acid and benzoic acid is 1:1~5:1~5; more preferably 1:2.18:2.18; by controlling The dosage ratio of each raw material can speed up the reaction and effectively improve the yield.
[0034] In yet another specific embodiment of the present invention, the specific conditions for heating to reflux are: react at 50-...
Embodiment 1
[0049] A preparation method of Bi-based metal-organic framework (Bi-MBA), the steps are as follows:
[0050] Add triphenylbismuth (51.6mg, 0.117mmol) and 4-mercaptobenzoic acid (39.2mg, 0.255mmol) into xylene (18mL), stir for 30min, and reflux at 60°C for 24h. Adding benzoic acid (31.1mg, 0.255mmol) as a regulator during the synthesis can obtain high-quality single crystals. After the reaction was sufficient, the yellow product was collected after cooling, filtering, washing (3 times with methanol and acetone), and drying (drying in an oven at 120° C. for 24 h). The yield was 82.3%.
[0051] Such as figure 1 As shown, Bi-MBA along the crystallographic a-axis is a one-dimensional Bi 2 S 4 Characterized by the crystal structure of the long chain, crystallized in the orthonormal space group Cmcm. Each Bi(III) is coordinated to one benzene ring of triphenylbismuth as a Bi source and four sulfur atoms in four ligand molecules, and Bi is pentacoordinated in Bi-MBA. Along the [...
Embodiment 2
[0055] Photoelectrochemical test:
[0056] The tests were performed in three-electrode mode using a 300 W xenon arc lamp (CEL-HFX300, CEAULIGHT) equipped with an AM1.5 filter as the light source. Catalyst-covered fluorine-doped tin oxide (FTO) glass, platinum sheet, Ag / AgCl and Na 2 SO 4 Solution (0.2mol L -1 ) as the working electrode, counter electrode, reference electrode and electrolyte, respectively. 50mg Bi-MBA samples were dispersed in 5mL ethanol, the suspension was spin-coated on FTO glass, and then dried at 70°C for 6h, the photocurrent density and electrochemical impedance spectroscopy were measured at 0V (vs Ag / AgCl) bias potential (EIS).
[0057] Such as Figure 5 As shown, under cut light and zero bias, Bi-MBA exhibits anodic photocurrent with a photocurrent density of about 0.03 μAcm -1 , indicating that Bi-MBA is an n-type semiconductor. It can be seen from the electrochemical impedance spectrum that the radius of Bi-MBA under light is smaller than that ...
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