Preparation method for superparamagnetic nanoparticle photocatalyst with Fe3O4-PAMAM-TiO2 core-shell structure

A technology of fe3o4-pamam-tio2 and nanoparticles, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc. Reduce the size of the magnetic particle, reduce the dispersion of magnetic particles, etc., to avoid the reduction of the specific surface area, slow down the oxidation and dissolution, and avoid the effect of particle aggregation

Inactive Publication Date: 2015-09-23
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heat treatment process will oxidize the magnetic core and reduce the saturation magnetic susceptibility; make TiO 2 The specific surface area decreases and the number of active hydroxyl groups decreases, which reduces the recyclability and catalytic activity of the photocatalyst
In addition, due to the bridging effect of linear polymers, the magnetic cores are prone to aggregation during the coating process, which increases the particle size and increases the hydrophobicity of the particle surface. After ultrasonic oscillation and grinding, the dispersion of the magnetic particles remains significantly decreased; and, polymers and inorganic minerals have completely different crystal structures, epitaxial growth of complete TiO on the surface of hydrophobic polymers 2 The crystal shell is very difficult, so it is difficult to obtain a monodisperse, magnetically supported photocatalyst with a complete core-shell structure

Method used

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  • Preparation method for superparamagnetic nanoparticle photocatalyst with Fe3O4-PAMAM-TiO2 core-shell structure

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Experimental program
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Effect test

Embodiment 1

[0021] Step (1): Superparamagnetic Fe 3 O 4 -Preparation of PAMAM nanoparticle colloidal solution: the concentration is 1×10 -5 The 6th-generation PAMAM dendrimers whose mol / L end groups are hydroxyl groups are filled with nitrogen and mechanically stirred for 60 minutes, then the iron salt mixture is added. The concentration of iron trichloride in the iron salt mixture is 1 mol / L , The concentration ratio of ferric chloride to ferric chloride is 2, and the amount of iron salt mixture added is Fe 3+ The ratio of the substance to the PAMAM dendrimer is 200:1 as the standard. Nitrogen is introduced at room temperature and stirred for 8 hours, then the temperature of the water bath is adjusted to 70℃, the stirring speed is increased to 800 rpm or more, and the concentration is 1 dropwise. ×10 -3 mol / L sodium hydroxide aqueous solution to pH 12, continue to stir for 60 min, then superparamagnetic Fe 3 O 4 -PAMAM nanoparticle colloidal solution.

[0022] Step (2): The surface is full...

Embodiment 2

[0026] Step (1): Superparamagnetic Fe 3 O 4 -Preparation of PAMAM nanoparticle colloidal solution: the concentration is 1×10 -5 The 6th-generation PAMAM dendrimer solution with the mol / L end group as ester group is filled with nitrogen and mechanically stirred for 40 minutes, and then the iron salt mixture is added. The concentration of iron trichloride in the iron salt mixture is 1 mol / L, the concentration ratio of ferric chloride to ferric chloride is 2, and the amount of iron salt mixture added is Fe 3+ The ratio of the substance to the PAMAM dendrimer is 120:1 as the standard. Nitrogen is introduced at room temperature and stirred for 6 hours, then the temperature of the water bath is adjusted to 80°C, the stirring speed is increased to 800 rpm or more, and the concentration is 1 dropwise. ×10 -2 mol / L sodium hydroxide aqueous solution to pH 11, continue to stir for 50 min, then superparamagnetic Fe 3 O 4 -PAMAM nanoparticle colloidal solution.

[0027] Step (2): The surfac...

Embodiment 3

[0031] Step (1): Superparamagnetic Fe 3 O 4 -Preparation of PAMAM nanoparticle colloidal solution: the concentration is 1×10 -4 The 5th-generation PAMAM dendrimer solution with carboxyl end groups in mol / L is filled with nitrogen and mechanically stirred for 30 minutes, then the iron salt mixture is added. The concentration of iron trichloride in the iron salt mixture is 1 mol / L , The concentration ratio of ferric chloride to ferric chloride is 1.5, and the amount of iron salt mixture added is Fe 3+ The ratio of the substance to the PAMAM dendrimer is 80:1 as the standard. Blow in nitrogen at room temperature and stir for 5 hours, then adjust the temperature of the water bath to 90℃, increase the stirring speed to 800 rpm or more, and drop the concentration to 1 ×10 -3 mol / L sodium hydroxide aqueous solution to pH 11, continue to stir for 40 min, then superparamagnetic Fe 3 O 4 -PAMAM nanoparticle colloidal solution.

[0032] Step (2): The surface is fully coated with Fe of PAMA...

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Abstract

The invention relates to a method for preparing a superparamagnetic nanoparticle photocatalyst with a Fe3O4-PAMAM-TiO2 core-shell structure by using polyamide-amine (PAMAM) dendrimer as a template and an isolation layer in a low-temperature aqueous solution. The method is characterized by comprising the following steps: firstly, with the PAMAM dendrimer as the template, preparing a superparamagnetic Fe3O4-PAMAM nanoparticle colloidal solution by using a co-precipitation method; then adding the PAMAM dendrimer with different terminal groups and coating Fe3O4-PAMAM nanoparticles so as to form a dendrimer isolation layer; finally, dropwise adding a TiCl4 absolute ethanol solution, and carrying out normal pressure reaction and hydrothermal reaction so as to obtain the nanoparticles with the Fe3O4-PAMAM-TiO2 core-shell structure and a complete TiO2 shell layer; and carrying out washing and redispersion so as to obtain the nanoparticle photocatalyst with the Fe3O4-PAMAM-TiO2 core-shell structure.

Description

technical field [0001] The invention relates to a superparamagnetic Fe 3 o 4 -PAMAM-TiO 2 The invention discloses a method for preparing a core-shell structure nano particle photocatalyst, belonging to the technical field of material preparation. Background technique [0002] With the development of modern industry, waste and residual chemical substances have caused serious threats to the environment and ecological safety, and people have to find effective ways to deal with these organic wastes. Photocatalysis is an advanced technology for degrading organic waste through oxidation reaction. It has achieved good results in oxidative degradation of azo dyes and pesticides. The current research focus is on how to effectively degrade various organic pollutants in water and air. . Nano-TiO 2 It has excellent photocatalytic activity, is cheap and non-toxic, has a band gap of 3.2eV, and exhibits excellent catalytic activity under ultraviolet light irradiation, and is considere...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38
Inventor 丛日敏于怀清杨思一
Owner SHANDONG UNIV OF TECH
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