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Preparation method of amino functional magnetic silicon dioxide adsorption material

An amino-functionalized, silica technology, applied in chemical instruments and methods, adsorption water/sewage treatment, alkali metal oxides/hydroxides, etc., can solve the problems of harsh conditions, complex operating processes, and high process conditions , to achieve the effect of fast adsorption kinetics, simplified preparation process and simple process

Inactive Publication Date: 2018-08-10
WUHAN UNIV OF TECH
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Problems solved by technology

Chinese patent document CN103721689A discloses the preparation method and application of the adsorbent of magnetic mesoporous silicon. The iron source and the silicon source are hydrolyzed at 110°C, roasted at 600°C, and then the magnetic SiO 2 Putting it into an organic solvent to make it oxidatively polymerize, and preparing a polyaniline-modified magnetic silica adsorbent and applying it to the adsorption of chromium ions in sewage; but this method has high requirements for process conditions, and organic solvents Toxic Serious Disadvantage
Similarly, the Chinese patent document CN105293783A discloses a treatment method for heavy metals in sewage, which prepares a hypophosphorous acid-modified magnetic silica composite material for the removal of zinc ions in wastewater; a Chinese patent document CN105771908A discloses a A magnetic silica core-shell composite material adsorbed by heavy metals is used to adsorb copper ions in wastewater and a ball technology modified magnetic mesoporous SiO disclosed in Chinese patent document CN106111071A for reducing heavy metal cadmium in wastewater 2 The preparation methods, etc., all adopt the first preparation of magnetic silica composite materials, and then PO in the organic solution by reflux method 2 h 2 , aminosilane, mercaptosilane, etc. to carry out graft modification, and use it to remove various heavy metal ions in wastewater; but they all use the method of first coating the magnetic core and then using the method of reflux for modification. The operation process is complicated, Disadvantages such as harsh conditions, high energy consumption and long reflux reaction time
Recently, Chinese patent document CN106861635 discloses a magnetic mesoporous silica adsorbent and its preparation method and its application in the treatment of combined pollution of organic matter and heavy metals in water. The magnetic core is prepared first, and then the silicon source precursor is The mixed reaction of solid and amine-based reagents is used to prepare adsorbents for adsorbing organic matter and heavy metal ions. However, because the silicon source is directly hydrolyzed in a strong alkaline solution, the silica coating layer is too thick, and there is only a small magnetic field. Disadvantages such as about 2.5emu / g are not conducive to rapid magnetic separation

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  • Preparation method of amino functional magnetic silicon dioxide adsorption material
  • Preparation method of amino functional magnetic silicon dioxide adsorption material
  • Preparation method of amino functional magnetic silicon dioxide adsorption material

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Effect test

Embodiment 1

[0035] (1) 2g FeCl 3 ·6H 2 O (analytical pure) was added to 60mL of ethylene glycol (analytical pure) and stirred until completely dissolved, then 3.5g CH 3 COONa (analytical pure), vigorously stirred for 30 min, then the mixture was transferred to a polytetrafluoroethylene kettle, and hydrothermally reacted at 180° C. for 12 h. Finally, the product is magnetically separated, washed several times with deionized water until the washing liquid is clear, washed once with ethanol (analytical pure), and dried at 60°C for 12 hours in a vacuum to obtain the magnetic Fe. 3 o 4 nanoparticles.

[0036] (2) Weigh the above Fe 3 o 4 Put 0.3g into the mixture of 3mL concentrated ammonia water (25-28%), 400mL ethanol (analytical pure) and 50mL distilled water, disperse under ultrasonic for 20min, then add dropwise 3mL tetraethyl orthosilicate (analytical pure), and stir the reaction After 1h, slowly add 300μL of 3-aminopropyltrimethoxysilane (97%) dropwise, continue to stir for 4h, a...

Embodiment 2

[0039] (1) 2g FeCl 3 ·6H 2 O (analytical pure) was added to 19 mL of ethylene glycol (analytical pure) and stirred until completely dissolved, then 2.4 g of CH 3 COONa (analytical grade) was vigorously stirred for 30 minutes, then the mixture was transferred to a polytetrafluoroethylene kettle, and hydrothermally reacted at 190° C. for 16 hours. Finally, the product is magnetically separated, washed several times with deionized water until the washing liquid is clear, washed once with ethanol (analytical pure), and dried at 60°C for 12 hours in a vacuum to obtain the magnetic Fe. 3 o 4 nanoparticles.

[0040] (2) Weigh the above Fe 3 o 4 Put 0.3g into a mixture of 3mL concentrated ammonia water (25-28%), 360mL ethanol (analytical pure) and 90mL distilled water, disperse under ultrasonic for 20min, then add dropwise 0.5mL tetraethyl orthosilicate (analytical pure), stir After reacting for 6 hours, slowly add 1100 μL of 3-aminopropyltriethoxysilane (99%) dropwise, continu...

Embodiment 3

[0043] (1) 2g FeCl 3 ·6H 2 O (analytical pure) was added to 74mL of ethylene glycol (analytical pure) and stirred until completely dissolved, then 3.6g CH 3 COONa (analytical pure), stirred vigorously for 30 min, then transferred the mixture to a polytetrafluoroethylene kettle, and reacted hydrothermally at 200° C. for 10 h. Finally, the product is magnetically separated, washed several times with deionized water until the washing liquid is clear, washed once with ethanol (analytical pure), and dried at 60°C for 12 hours in a vacuum to obtain the magnetic Fe. 3 o 4 nanoparticles.

[0044] (2) Weigh the above Fe 3 o 4 Put 0.3g into a mixture of 3mL concentrated ammonia water (25-28%), 405mL ethanol (analytical grade) and 45mL distilled water, disperse under ultrasonic for 20min, then add dropwise 4mL tetraethyl orthosilicate (analytical grade), and stir to react After 0.4h, slowly add 300μL of N-(aminoethyl)-γ-aminopropyltrimethoxysilane (95%) dropwise, continue to stir ...

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Abstract

The invention discloses a preparation method of an amino functional magnetic silicon dioxide adsorption material. The method comprises the following preparation process that firstly, solid Fe3O4 nanoparticles are prepared by a solvothermal method; then, the solid Fe3O4 nano particles are put into a mixed solution of absolute ethyl alcohol and water; a certain quantity of ammonia water is added; after ultrasonic dispersion, ethyl orthosilicate is added drop by drop at normal temperature; after stirring reaction is performed for a period of time, a certain quantity of different kinds of amino-silane coupling agents are added; continuous stirring is performed for reaction for a period of time; after the product is subjected to magnetic separation, washing and vacuum drying, an amino functional Fe3O4@SiO2 composite adsorbing material with a core-shell structure is prepared. The prepared amino functional Fe3O4@SiO2 composite adsorbing material has good adsorption performance on virulent contaminants Cr(VI) in wastewater; particularly, the significant advantages of fast adsorption kinetics is realized; after one-hour adsorption, the adsorption is balanced; the characteristic of fast separation after the adsorbent adsorbs the contaminants is realized.

Description

technical field [0001] The present invention relates to the technical field of the preparation of magnetic silica composite materials, more precisely an amino-functionalized Fe used for the adsorption of highly toxic pollutants Cr(VI) in water 3 o 4 @SiO 2 Preparation and application of core-shell structured adsorbents. Background technique [0002] Toxic heavy metal ions are one of the main causes of environmental pollution, especially in water resources. In recent years, water pollution caused by metal ions has attracted widespread attention because of their carcinogenicity, mutagenicity, genotoxicity, and bioaccumulation through the food chain, etc., causing serious health and environmental problems. Among them, chromium is a typical element, which exists in different oxides and has different degrees of toxicity to the environment and the toxicity of humans, animals and plants. The main sources of Cr(VI) pollution are directly related to electroplating, steel, textile...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/28B01J20/30C02F1/28C02F101/22
CPCB01J20/06B01J20/103B01J20/28009B01J2220/4806B01J2220/4812C02F1/281C02F2101/22
Inventor 蔡卫权古蒙蒙
Owner WUHAN UNIV OF TECH
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