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C12-to-C18 alkyl phosphonic acid protection magnetic ferroferric oxide nanocrystalline as well as preparation method and application thereof

A technology of triiron tetroxide and alkyl phosphonic acid, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effect of simple process

Inactive Publication Date: 2012-03-21
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For nanoparticles with a particle size of less than 50 nm, traditional catalyst separation methods such as filtration and centrifugation are difficult to completely separate the catalyst from the liquid phase system

Method used

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  • C12-to-C18 alkyl phosphonic acid protection magnetic ferroferric oxide nanocrystalline as well as preparation method and application thereof
  • C12-to-C18 alkyl phosphonic acid protection magnetic ferroferric oxide nanocrystalline as well as preparation method and application thereof
  • C12-to-C18 alkyl phosphonic acid protection magnetic ferroferric oxide nanocrystalline as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Prepare 10 mL of 1.5 mol / L ferrous chloride aqueous solution, and then prepare 0.015 mol / L hexadecylphosphonic acid solution with a mixed solution of 15 mL of distilled water and 5 mL of ethanol. The hexadecylphosphonic acid solution was slowly added to the ferrous chloride solution and stirred for 60 min, and the pH value of the mixed solution was adjusted to 5.0 with concentrated ammonia water. The above prepared mixed solution was transferred to a 50mL stainless steel autoclave, treated at 180°C for 24h, and cooled naturally. Separation of magnetic Fe using a magnet 3 o 4 product, such as Figure 13 shown. Vacuum dried at 40°C. The obtained product was identified as Fe by X-ray powder diffraction 3 o 4 ,Such as Figure 8 shown. The alkylphosphonic acid coated on its surface was characterized by thermogravimetric analysis and infrared spectroscopy, such as Figure 9 and Figure 12 shown. Using transmission electron microscopy to characterize its morphology,...

Embodiment 2

[0041] Prepare 10 mL of 1.5 mol / L ferrous chloride aqueous solution, and then prepare 0.015 mol / L dodecylphosphonic acid solution with a mixed solution of 15 mL of distilled water and 5 mL of ethanol. The dodecylphosphonic acid solution was slowly added to the ferrous chloride solution and stirred for 60 min, and the pH value of the mixed solution was adjusted to 5.0 with concentrated ammonia water. The above prepared mixed solution was transferred to a 50mL stainless steel autoclave, treated at 180°C for 24h, and cooled naturally. Separation of magnetic Fe using a magnet 3 o 4 The product was dried under vacuum at 40°C. The obtained product was identified as Fe by X-ray powder diffraction 3 o 4 , characterized by thermogravimetric analysis and infrared spectroscopy of the alkyl phosphonic acid coated on its surface, and its morphology was characterized by transmission electron microscopy, such as figure 2 shown. 0.1 g of the prepared alkylphosphonic acid protected Fe ...

Embodiment 3

[0043] Prepare 10 mL of 1.5 mol / L ferrous sulfate aqueous solution, and then prepare 0.015 mol / L octadecylphosphonic acid solution with a mixed solution of 15 mL of distilled water and 5 mL of ethanol. The octadecylphosphonic acid solution was slowly added to the ferrous sulfate solution and stirred for 60 min, and the pH value of the mixed solution was adjusted to 5.0 with concentrated ammonia water. The above prepared mixed solution was transferred to a 50mL stainless steel autoclave, treated at 180°C for 24h, and cooled naturally. Separation of magnetic Fe using a magnet 3 o 4 The product was dried under vacuum at 40°C. The obtained product was identified as Fe by X-ray powder diffraction 3 o 4 , characterized by thermogravimetric analysis and infrared spectroscopy of the alkyl phosphonic acid coated on its surface, and its morphology was characterized by transmission electron microscopy, such as image 3 shown. 0.1 g of the prepared alkylphosphonic acid protected Fe...

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Abstract

The invention provides a C12-to-C18 alkyl phosphonic acid protection magnetic ferroferric oxide nanocrystalline. The diameter of the magnetic ferroferric oxide nanocrystalline is 10 to 100nm, and the surface of the magnetic ferroferric oxide nanocrystalline is covered with C12 to C18 alkyl phosphonic acid. The invention also provides a preparation method of the nanocrystalline and an application of the nanocrystalline as catalysts to the preparation of benzaldehyde through toluene oxidation. The whole process is simple, the nanocrystalline is applicable to large-scale production, in addition, economy is realized, and no pollution is caused. The nanocrystalline provided by the invention has higher conversion rate and selectivity when being used as the catalyst under the certain reaction condition, the simple and full separation can be realized by magnetism after the reaction completion, the repeated use is realized, and in addition, the conversion rate and the selectivity maintain unchanged.

Description

technical field [0001] The present invention relates to C 12 ~C 18 Alkylphosphonic acid-protected magnetic ferric iron tetraoxide nanocrystals, its preparation method and its application as a catalyst in the selective oxidation reaction of benzaldehyde prepared by liquid-phase selective oxidation of toluene. Background technique [0002] The most important goal of heterogeneous catalysis is to design catalysts with high selectivity to target products without compromising their activity. In recent years, it has been found that nanomaterials with special structure and morphology can effectively solve this problem. For example, Yang Peidong confirmed that platinum nanocubes have high selectivity for pyrrole hydrogenation. Lu Gaoqing also found that the preferentially exposed {001} facet of titanium oxide has high photocatalytic activity. Ding Weiping using C 12 ~C 18 Carboxylate-protected cerium oxide nanocrystals have high selectivity and activity for the direct oxidation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J33/00C07C47/54C07C45/36
Inventor 丁维平李磊纪文旭李明起沈逸吕建刚郭学锋彭路明薛念华
Owner NANJING UNIV
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