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Preparation method of spherical Fc-(COOH)2@COFETTA-TPAL nano composite

A technology of nanocomposite materials and mixed solutions, applied in the field of material chemistry, can solve the problems of restricting the wide use of materials and single performance, and achieve the effect of rapid and sensitive detection and avoiding agglomeration

Active Publication Date: 2018-10-09
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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  • Preparation method of spherical Fc-(COOH)2@COFETTA-TPAL nano composite
  • Preparation method of spherical Fc-(COOH)2@COFETTA-TPAL nano composite
  • Preparation method of spherical Fc-(COOH)2@COFETTA-TPAL nano composite

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Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0023] (2) Add 0.2 mL of 6M 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 hours 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 hours, and then ground to obtain a khaki solid Fc-(COOH) 2 @COF ETTA-TPAL composite material.

Embodiment 2

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

[0027] (2) Add 0.2 mL of 6M 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 for 11 hours in a mixed solution with an alkane volume ratio of 1:1 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 hours, and then ground to obtain a khaki solid Fc-(COOH) 2 @COF ETTA-TPAL composite material.

Embodiment 3

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

[0031] (2) Add 0.2 mL of 6M 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 hours 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 hours, and then 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 novel method to prepare spherical covalent framework material (COFETTA-TPAL) nano composite (Fc-(COOH)2@COFETTA-TPAL) with electroactive ferrocenecarboxylic acid molecules (Fc-(COOH)2). Tetra-(4-aminobenzene)ethylene (ETTA), terephthalaldehyde (TPAL) and Fc-(COOH)1 are co-dissolved in 1,4-dioxane solvent before ultrasonic mixing; acetic acid is added; the mixed solution is transferred to a reactor and allowed to react in an oven at 120 DEG C for 2 days so as to obtain earthy yellow solid Fc-(COOH)2@COFETTA-TPAL nano composite. The Fc-(COOH)2@COFETTA-TPAL nano composite prepared via solvothermal one-pot synthesis is spherical, with uniform size and diameter of about 200 nm. Fc-(COOH)2 Molecules are well loaded in holes of COFETTA-TPAL. Crystal structure of the COFETTA-TPAL is well maintained, and electroactivity of Fc-(COOH)2 and COFETTA-TPAL is retained. Studies discover that the nano composite can catalyze disproportionation reaction of H2O2 and may replace peroxidase, the preparation process is simple, and the materials are low in price 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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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
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