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Preparation method and application method of bispyridylamide iron-supported nano-silica heterogeneous catalyst
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A nano-silica, iron bispyridine amide technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve pH sensitivity, instability, Low activity and other problems, to achieve the effect of improving dispersibility, improving efficiency, and simple synthesis method
Active Publication Date: 2022-03-04
HARBIN INST OF TECH
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[0003] The purpose of the present invention is to solve the technical problem that Fedpa is sensitive to pH, and is prone to polymerization or demetallization in neutral and acidic water bodies, thus showing low activity and instability, and provides a bispyridylamide iron-loaded nanometer Preparation method and application method of silica heterogeneous catalyst
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specific Embodiment approach 1
[0033] DETAILED DESCRIPTION an: embodiment of the present method for preparing iron-bipyridine amide nano-silica supported heterogeneous catalyst in accordance with the following steps:
[0034] I. Synthesis of nano-SiO 2 ;
[0035] Second, the nano-SiO 500mg 2 Ultrasonic dispersion in 100mL of anhydrous tetrahydrofuran to give SiO 2 The suspension was 2mL3- aminopropyl triethoxysilane was added dropwise to a magnetic stirring rate of 1000rpm SiO 2 The suspension was refluxed in an oil bath of 100 deg.] C for 6 hours, isolated by filtration, washed three times with acetonitrile, washed three times with de-ionized water, at a temperature of 60 ℃ dried, aminated surface obtained nanosilica SiO 2 -NH 2 ;
[0036] Third, the carboxylic acid 4.2 g of 2- -N, phthalic two N`- - (2-pyridin-formyl) - amine and mixing iron complex of anhydrous tetrahydrofuran 40mL, 1.0g of triethylamine was added dropwise, in a nitrogen atmosphere 1.1g of ethyl chloroformate was added dropwise, the reaction...
specific Embodiment approach 2
[0038] DETAILED Embodiment 2: Embodiment of the present embodiment and the exemplary embodiment except that a step in the synthesis of a nano-silica material SiO 2 The method is as follows:
[0039] (1) preparing a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water is 1: 1;
[0040] (2) the tetraethylorthosilicate (TEOS) was added dropwise to a magnetic stirring rate of 1000rpm in step (1) a mixed solution obtained was stirred for 30 min;
[0041] (3) Aqueous ammonia was added to a magnetic stirring rate of 1000rpm in step (2) to obtain a mixture of the pH of the mixture is from 10 to 11, stirred for 6 hours, to obtain SiO 2 suspension;
[0042] (4) A SiO 2 The suspension was separated by centrifugation, washed with deionized water SiO 2 Supernatant to solid neutral, and then SiO2 The solid was dried at 60 ℃ to obtain nano-silica material SiO 2 . Other specific embodiments of a same.
specific Embodiment approach 3
[0043] DETAILED Embodiment 3: Embodiment of the present embodiment and the exemplary embodiment one or two different reaction stirred for 50 minutes in an ice-water bath in step three. Other specific embodiments of the same one or two.
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Abstract
A preparation method and an application method of a bispyridylamide iron-supported nano-silica heterogeneous catalyst relate to a preparation method and an application method of a catalyst. The present invention is to solve the problem that Fedpa is sensitive to pH, prone to polymerization or demetallization in neutral and acidic waters, and exhibits low activity and instability. The method is as follows: Synthesis of nano-silica material SiO 2 ; Preparation of surface aminated nano-silica SiO 2 ‑NH 2 ; Synthesis of bispyridine amide iron complex with ethyl anhydride substituent; Disperse the synthesized bispyridyl amide iron complex with ethyl anhydride substituent on the surface amino group-modified silica SiO 2 ‑NH 2 in tetrahydrofuran solution. The invention immobilizes the Fedpa, thereby realizing the isolation of the Fedpa molecules and improving the reusability of the Fedpa. The composite material is more stable because the immobilized material is connected to the carrier material by chemical bonding. The invention belongs to the field of catalyst preparation.
Description
Technical field [0001] The present invention relates to a method of preparation and use of a catalyst. Background technique [0002] Bipyridine amide Fedpa iron can activate hydrogen peroxide efficiently and quickly degrading 2,4-DCP, so it can be used to degrade the waste water containing the 2,4-DCP. Currently, bipyridine amide iron have been found capable of degrading endocrine disruptors (bisphenol A and tetrabromobisphenol A), organochlorine pesticides (p-chlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) and dye . Since Fedpa sensitive to pH, water at neutral and acidic or readily polymerized demetallization exhibit the phenomenon of instability and low activity. Inventive content [0003] Object of the present invention is to solve the Fedpa sensitive to pH, water at neutral and acidic or readily polymerized demetallization phenomena exhibit low activity and instability technical problems, there is provided a dual load nano-pyridine carboxamide Fe preparation of s...
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