Preparation and application of Tb-MOF nanosheets based on pyrene tetracarboxylic acid

A pyrene tetracarboxylic acid and nanosheet technology is applied in the field of pyrene tetracarboxylic acid-based Tb-MOF nanosheets and their preparation, which can solve problems such as adverse effects on the environment, and achieve increased direct contact area, simple operation, and easy access. Effect

Pending Publication Date: 2021-09-21
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional method of obtaining sulfoxide in the early stage is to use strong oxidants, such as strong acids, iodic acid, hydroperoxides, nitrogen oxides, etc. However, the waste generated by these oxidants in the post-processing process will have many adverse effects on the environment

Method used

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  • Preparation and application of Tb-MOF nanosheets based on pyrene tetracarboxylic acid
  • Preparation and application of Tb-MOF nanosheets based on pyrene tetracarboxylic acid
  • Preparation and application of Tb-MOF nanosheets based on pyrene tetracarboxylic acid

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preparation example Construction

[0032] Such as figure 1 Shown, the preparation method of the Tb-MOF nanosheet based on pyrene tetracarboxylic acid of the present invention, it comprises the steps:

[0033] 1) Dissolve 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene, terbium acetate hexahydrate or terbium nitrate hexahydrate at a molar ratio of 1:3 in an equal volume of N,N-dimethyl 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution and terbium acetate or terbium nitrate solution were obtained by ultrasonication at 100 Hz until it was completely dissolved in acetamide;

[0034] 2) Mix equal volumes of 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution, terbium acetate solution or terbium nitrate solution obtained in step 1) in a glass bottle, add acid to adjust, and then 100Hz ultrasonic for 10min It is well mixed;

[0035] 3) Put the mixed glass bottle into a microwave oven, react at 400-500W for 5-10min, cool to room temperature, collect the precipitate after centrifugation at 10000r / min, and wash twice with N,N-dime...

Embodiment 1

[0041] (a) Dissolve 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene (20.54 mg, 0.03 mmol) and terbium acetate hexahydrate (31.25 mg, 0.09 mmol) in 5 mL of N,N-di In methyl acetamide, sonicate at 100 Hz for ten minutes until it is completely dissolved to obtain 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution and terbium acetate solution;

[0042](b) Mix 100 µL each of the obtained 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution and terbium acetate solution in a 3 mL glass bottle, dilute to 1 mL, and then add 5 µL (0.09 mmol) acetic acid , 10min ultrasonic at 100Hz to mix it evenly;

[0043] (c) Put the glass bottle in a microwave oven, react at 400W for five minutes, cool to room temperature, centrifuge at 10,000r / min to collect the precipitate, wash twice with N,N-dimethylacetamide and ethanol, then disperse in water and place in Freeze-drying in a freeze dryer for 24 h yielded 0.38 mg of Tb-MOF nanosheets, and the yield of the obtained nanosheets was 92% (compared to the ligand). ...

Embodiment 2

[0046] (a) Dissolve 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene (20.54 mg, 0.03 mmol) and terbium acetate hexahydrate (31.86 mg, 0.09 mmol) in 5 mL of N,N-di In methyl acetamide, sonicate at 100 Hz for ten minutes until it is completely dissolved to obtain 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution and terbium acetate solution;

[0047] (b) Mix 100 µL each of the obtained 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene solution and terbium acetate solution in a 3 mL glass bottle, dilute to 1 mL, and directly sonicate at 100 Hz without adding acid 10min to mix it evenly;

[0048] (c) Put the glass bottle in a microwave oven, react at 400W for five minutes, cool to room temperature, centrifuge at 10,000r / min to collect the precipitate, wash twice with N,N-dimethylacetamide and ethanol, then disperse in water and place in Freeze-drying in a freeze dryer for 24 h yielded 0.37 mg of Tb-MOF nanosheets, and the yield of the obtained nanosheets was 90% (compared to the ligand).

[0049] T...

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Abstract

The invention discloses a preparation method and application of Tb-MOF nanosheets based on pyrene tetracarboxylic acid. The preparation method comprises the following steps of: respectively dissolving 1, 3, 6, 8-tetra (4-carboxybenzene) pyrene and terbium acetate hexahydrate or terbium nitrate hexahydrate in N, N-dimethylacetamide, carrying out ultrasonic treatment to completely dissolve the 1, 3, 6, 8-tetra (4-carboxybenzene) pyrene and terbium acetate hexahydrate or terbium nitrate hexahydrate, and then carrying out ultrasonic uniform mixing on two solutions; and preparing the Tb-MOF nanosheets by a microwave synthesis method. The Tb-MOF nanosheets obtained by the method of the invention can realize efficient and high-selectivity catalytic oxidation of thioether organic matters into corresponding sulfoxide compounds in green solvents (water, acetonitrile and methanol), and have a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a pyrene tetracarboxylic acid-based Tb-MOF nanosheet and a preparation method and application thereof. Background technique [0002] The selective oxidation of sulfides to sulfoxides or sulfones has important applications in biomedicine and has aroused great interest in the fields of organic chemistry and synthetic chemistry, especially the intermediates of sulfoxides, which are widely used in biology, medicine, oxidative desulfurization and industry fields of chemistry. The traditional method of obtaining sulfoxide in the early stage is to use strong oxidants, such as strong acids, iodic acid, hydroperoxides, nitrogen oxides, etc. However, the waste generated during the post-processing of these oxidants will have many adverse effects on the environment. The preparation of a more environmentally friendly and efficient catalyst that can directly catalyze oxidation i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10B01J37/34C08G83/00C07C315/02C07C317/14C07C317/22
CPCB01J31/1691B01J31/2239B01J35/004B01J35/023B01J35/1014B01J35/1019B01J35/1023B01J37/346C08G83/008C07C315/02B01J2531/0216B01J2531/38B01J2231/70C07C317/14C07C317/22
Inventor 庄金亮冯丽
Owner GUIZHOU NORMAL UNIVERSITY
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