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Surface-aminated Fe3O4 nano particle and preparation method and application thereof

A technology of surface amination and nano-particles, applied in chemical instruments and methods, inorganic chemistry, ion exchange, etc., can solve the problems of long reaction time, poor particle shape and complicated preparation process of coprecipitation method, and shorten the time Effects of processing time, improving efficiency, and simplifying steps

Inactive Publication Date: 2013-03-27
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all have different disadvantages. The coprecipitation method takes too long to react, the hydrothermal method lies in the poor shape of the particles, the template method lies in the complicated preparation process of the template, and the organic phase reduction method lies in the low yield.

Method used

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  • Surface-aminated Fe3O4 nano particle and preparation method and application thereof
  • Surface-aminated Fe3O4 nano particle and preparation method and application thereof
  • Surface-aminated Fe3O4 nano particle and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Embodiment 1, aminated magnetic Fe 3 o 4 Synthesis of Nanoparticles

[0045] (1) Magnetic Fe 3 o 4 Synthesis of Nanoparticles

[0046] Pass nitrogen gas into a 500mL Erlenmeyer flask for about 20min, then add 2gFeCl to it in sequence 2 4H 2 O, 5.2 g FeCl 3 ·6H 2 O. Dissolve 0.85mL of 12mol / L hydrochloric acid in 200mL of water, and ultrasonically deoxygenate for 20min. Prepare 250mL of 0.75mol / L sodium hydroxide solution and ultrasonically deoxygenate for 20min. Add the prepared hydrochloric acid solution and sodium hydroxide solution to the Erlenmeyer flask in turn, put in the magnet, and pass nitrogen gas again for about 10 minutes to ensure that the Erlenmeyer flask is filled with nitrogen, and quickly cover the Erlenmeyer flask with the cap and seal it. In the environment of the water bath of 80 ℃, electromagnetic stirring was reacted for 2h, and black precipitate was obtained. Separated with an external magnetic field, washed 3 times with deionized water...

Embodiment 2

[0050] Embodiment 2, aminated magnetic Fe 3 o 4 Synthesis of Nanoparticles

[0051] (1) Take about 0.7g of 2mmol of iron (III) acetylacetonate, about 2.6g of 10mmol of 1,2-hexadecane diol, about 20mL of diphenyl ether or dibenzyl ether, about 2.6ml of 6mmol of oleyl ammonia , 6mmol of oleic acid, about 2.6mL, was put into a three-neck flask. In order to prevent the oxidation of the medicine, nitrogen gas should be passed for 20 minutes before adding the medicine. Under the condition of nitrogen protection, be heated to 200 ℃ with the speed of 10 ℃ per minute, react 1h, be heated to 260 ℃ again, react 30min. Stop heating, let it return to room temperature, add 40 mL of ethanol to the reaction solution, and centrifuge at a speed of 10000 r / min for 20 min in a centrifuge to obtain a black precipitate. Discard the supernatant, and wash the black precipitate with absolute ethanol 2-3 times to obtain magnetic Fe 3 o 4 Nanoparticles. will get Fe 3 o 4 The nanoparticles are di...

Embodiment 3

[0054] Embodiment 3, aminated magnetic Fe 3 o 4 Performance testing of nanoparticles

[0055] (1) TEM analysis

[0056] In order to determine the size of the prepared particles and overcome the agglomeration of the solid sample during electron microscope detection, the prepared magnetic Fe 3 o 4 Nanoparticles and their magnetic Fe after amination 3 o 4 The nanoparticles are fully dispersed with n-hexane, the sample is dropped on the copper grid, and the scanning detection of the transmission electron microscope is carried out. The transmission electron microscope image (TEM) is as follows: figure 1 shown. As can be seen from the picture, the magnetic Fe synthesized in the organic phase (Example 2) 3 o 4 Nanoparticles present obvious regular hexahedral shape, particle size is consistent, all about 50nm, neatly arranged, showing the arrangement rule of superlattice. Inorganic Phase Synthesis (Example 1) of Magnetic Fe 3 o 4 Compared with the particles synthesized in t...

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Abstract

The invention discloses a surface-aminated Fe3O4 nano particle and a preparation method and the application thereof. The method comprises the following steps: (1) in inert atmosphere, FeCl2 and FeCl3 are added into the mixed solution of sodium hydroxide aqueous solution and hydrochloric acid aqueous solution for reaction and Fe3O4 nano particles are obtained; (2) ethanol solution of the Fe3O4 nano particles is prepared; in inert atmosphere, strong ammonia water and tetraethoxysilane are added into the ethanol solution of the Fe3O4 nano particles and after reaction, modified Fe3O4 nano particles are obtained; and (3) the ethanol solution of the Fe3O4 nano particles with a good dispersion effect is prepared; in inert atmosphere, 3-aminopropyl triethoxy silane is added into the ethanol solution of the modified Fe3O4 nano particles and after reaction, the surface-aminated Fe3O4 nano particles are obtained. The aminated Fe3O4 nano particles provided by the invention can have good adsorption capacity to 5 types of phenylarsonic acid at the same time. At the same time, as the aminated Fe3O4 nano particles have superparamagnetism, centrifugalization is unnecessary for sample treatment. Thus, the steps of pretreatment of samples are greatly simplified, the pretreatment time is shortened and the efficiency of the pretreatment of samples is increased.

Description

technical field [0001] The invention relates to a surface aminated Fe 3 o 4 Nanoparticles and their preparation methods and applications. Background technique [0002] Phenylarsenic acid is a kind of feed additive that is commonly used. It belongs to non-nutritive growth-promoting and health-care antibiotics. It can be synthesized by chemical methods. Adding phenylarsenic acid to feed can play a very good role in sterilization and antibacterial Effect. Phenylarsenate exists in various forms, including p-aminophenylarsenic acid (APAA), p-hydroxyphenylarsenic acid (p-HPAA), p-nitrophenylarsenic acid (NPAA), p-amidophenylarsenic acid (AAPAA) and Roxars (Rox) et al. [0003] Magnetic Fe 3 o 4 Nanoparticles have been widely used in the enrichment process of arsenic. Wu Shaoxiong, Xing Zhi et al. utilize magnetic Fe 3 o 4 Nanoparticles selectively enrich arsenic in water, in the range of pH2-10, Fe 3 o 4 It can quantitatively enrich As(V), As(III), MMA and DMA, the line...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01J20/28B01D15/08
Inventor 苏晓鸥王培龙朱若华李然张维李阳王瑞国
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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