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Spherical fc-(cooh) 2 @cof etta-tpal Preparation methods of nanocomposites

A nano-composite material and mixed solution technology, applied in the field of material chemistry, can solve the problems of single performance and limit the wide use of materials, and achieve the effect of rapid and sensitive detection and avoidance of agglomeration

Active Publication Date: 2022-03-04
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since it is insoluble in water and most organic solvents (such as acetone, methanol, acetone, tetrahydrofuran, DMF, dimethyl sulfoxide, etc.), the normally synthesized COF ETTA-TPAL Often agglomerated together, and the performance is relatively single, which further limits the wide use of this material

Method used

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  • Spherical fc-(cooh)  <sub>2</sub> @cof  <sub>etta-tpal</sub> Preparation methods of nanocomposites
  • Spherical fc-(cooh)  <sub>2</sub> @cof  <sub>etta-tpal</sub> Preparation methods of nanocomposites
  • Spherical fc-(cooh)  <sub>2</sub> @cof  <sub>etta-tpal</sub> Preparation methods of nanocomposites

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Dissolve 22 mg ETTA (10 mg / mL), 15 mg (6.85 mg / mL) TPAL and 11 mg (5 mg / mL) ferrocenedicarboxylic acid in 2 mL 1,4-dioxane solvent, and ultrasonically mixed for 15 min;

[0023] (2) Add 0.2 mL of 6 M acetic acid solution to the mixed solution. Transfer the mixed solution to a reaction kettle and place it in an oven at 90°C for 2 days;

[0024] (3) Use N,N-dimethylformamide (DMF) and tetrahydrofuran (THF) as solvents to successively centrifuge the obtained precipitate until the supernatant is colorless, then place the precipitate in THF and dichloroethane Soak in the mixed solution with a volume ratio of 1:1 for 10 h in order to more fully remove the organic monomer molecules and impurities adsorbed by the precipitate. Finally, the precipitate was dried in a vacuum freeze dryer for 24 h, and ground to obtain a khaki solid Fc-(COOH) 2 @COF ETTA-TPAL composite material.

Embodiment 2

[0026] (1) Dissolve 30 mg ETTA (13.64 mg / mL), 20.5 mg (9.32 mg / mL) of TPAL and 22 mg (10 mg / mL) of ferrocenedicarboxylic acid in 2 mL of 1,4-dioxo Hexacyclic solvent, and ultrasonically mixed for 15 min;

[0027] (2) Add 0.2 mL of 6 M acetic acid solution to the mixed solution. Transfer the mixed solution to a reaction kettle and place it in an oven at 100°C for 2 days;

[0028] (3) Use N,N-dimethylformamide (DMF) and tetrahydrofuran (THF) as solvents to successively centrifuge and wash the obtained precipitate until the supernatant is colorless, and then place the precipitate in THF and dichloroethane Soak in a mixed solution with an alkane volume ratio of 1:1 for 11 h in order to more fully remove the organic monomer molecules and impurities adsorbed by the precipitate. Finally, the precipitate was dried in a vacuum freeze dryer for 24 h, and ground to obtain a khaki solid Fc-(COOH) 2 @COF ETTA-TPAL composite material.

Embodiment 3

[0030] (1) Dissolve 33 mg ETTA (15 mg / mL), 22.5 mg TPAL (10.25 mg / mL) and 55 mg (25 mg / mL) of ferrocenedicarboxylic acid in 2 mL of 1,4-dioxane solvent, and ultrasonically mixed for 15 min;

[0031] (2) Add 0.2 mL of 6 M acetic acid solution to the mixed solution. Transfer the mixed solution to a reaction kettle and place it in an oven at 120°C for 2 days of reaction;

[0032] (3) Use N, N-dimethylformamide (DMF) and tetrahydrofuran (THF) as solvents to successively centrifuge the obtained precipitate until the supernatant is colorless, then place the precipitate in THF and dichloroethane Soak in the mixed solution with a volume ratio of 1:1 for 12 h in order to more fully remove the organic monomer molecules and impurities adsorbed by the precipitate. Finally, the precipitate was dried in a vacuum freeze dryer for 24 h, and ground to obtain a khaki solid Fc-(COOH) 2 @COF ETTA-TPAL composite material.

[0033] Fc-(COOH) prepared by the above-mentioned solvothermal one-pot...

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Abstract

The invention discloses a method for preparing and wrapping electroactive ferrocene dicarboxylic acid molecules (Fc-(COOH) 2 ) spherical covalent organic frameworks (COF ETTA‑TPAL ) nanocomposite (Fc‑(COOH) 2 @COF ETTA‑TPAL ) of the new method. By combining tetra-(4-aminobenzene)ethylene (ETTA), terephthalaldehyde (TPAL) and Fc-(COOH) 2 Dissolve together in 1,4‑dioxane solvent, mix ultrasonically and then add acetic acid, and finally transfer the mixture to a reaction kettle and place it in an oven at 120°C for 2 days to obtain a khaki solid Fc‑(COOH) 2 @COF ETTA‑TPAL nanocomposites. Fc‑(COOH) Prepared by Solvothermal One-Pot Synthesis 2 @COF ETTA‑TPAL The nanocomposite is spherical and uniform in size, with a diameter of about 200nm. Fc‑(COOH) 2 Molecules are well loaded in COF ETTA‑TPAL in the hole. better maintained COF ETTA‑TPAL The crystal structure of the material while retaining the Fc‑(COOH) 2 with COF ETTA‑TPAL electroactive properties. The study found that the nanocomposite can catalyze H 2 o 2 The disproportionation reaction occurs, and the peroxidase can be replaced, the preparation process is simple, and the raw materials are cheap and easy to obtain.

Description

technical field [0001] The invention relates to a method for preparing uniform spherical Fc-(COOH) 2 @COF ETTA-TPAL A method for a nanocomposite material belongs to the field of materials chemistry. Background technique [0002] Covalent organic framework (COF) is a new type of material developed after inorganic zeolite-like porous materials and metal-organic framework (MOF). It is a new type of crystalline porous polymer material with a relatively stable structure. Pore ​​size distribution, large specific surface area and many special functional groups, easy to load a variety of functional small molecules or protein molecules. COF ETTA-TPAL It is obtained by condensation reaction of tetra-(4-aminophenyl)ethylene (ETTA) and terephthalaldehyde (TPAL) at high temperature through ammonia aldehyde. It is a typical two-dimensional lamellar stacked porous material, which is relatively stable at high temperature, thereby overcoming the defects of single composition, uneven dist...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J37/34B01J37/10B01J37/03B82Y30/00B82Y40/00G01N27/48
CPCG01N27/48B82Y30/00B82Y40/00B01J31/1691B01J31/2295B01J37/031B01J37/10B01J37/343B01J35/396B01J35/33
Inventor 宋永海汪莉徐孟丽梁慧慧
Owner JIANGXI NORMAL UNIV