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A continuous flow process for manufacturing surface modified metal oxide nanoparticles by supercritical solvothermal synthesis

A nanoparticle, surface modification technology, applied in the process of supercritical conditions, chemical instruments and methods, titanium oxide / hydroxide, etc., can solve the problem of not allowing to control the size distribution of nanoparticles or control the function of nanoparticles the way of transformation, etc.

Inactive Publication Date: 2017-10-20
ESSILOR INT CIE GEN DOPTIQUE +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this approach does not allow control over the size distribution of the nanoparticles or control over the way the nanoparticles are functionalized

Method used

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  • A continuous flow process for manufacturing surface modified metal oxide nanoparticles by supercritical solvothermal synthesis
  • A continuous flow process for manufacturing surface modified metal oxide nanoparticles by supercritical solvothermal synthesis
  • A continuous flow process for manufacturing surface modified metal oxide nanoparticles by supercritical solvothermal synthesis

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0117] Example 1: TiO 2 Functionalization of nanoparticles

[0118] figure 1 A schematic of the continuous flow reactor system is shown.

[0119] ROH = ethanol

[0120] HPP = high pressure pump

[0121] P = pressure gauge

[0122] V = valve

[0123] Vr = regulating valve, also known as back pressure regulator

[0124] F = filter

[0125] C = condenser

[0126]The system comprises four modules R1 to R4 connected in series. R1 and R2 are the hydrolysis modules used to perform this hydrothermal synthesis under subcritical conditions. R3 and R4 are supercritical modules for performing this hydrothermal synthesis under supercritical conditions.

[0127] The injection point of the surface modifier is positioned before reactor R1, between the different modules (R1-R2, R2-R3, R3-R4) and after reactor R4.

[0128] TiO was carried out in a mixture of water and ethanol (water / ethanol molar ratio = 0.8) under the following conditions 2 Supercritical Hydrothermal Synthesis o...

example 2

[0163] Example 2: ZrO 2 Functionalization of nanoparticles

[0164] Use the same system as the system used in Example 1, prepare ZrO with the same operating conditions 2 Microcrystalline.

[0165] Reactant:

[0166] -Zr precursor: zirconium acetylacetonate, zirconium acetate, zirconium propoxide or zirconium isopropoxide.

[0167] - Surface modifiers: caproic acid, octylphosphonic acid, phenylphosphonic acid, phosphorous acid or SIK7709-10 (12-dodecylphosphonic acid) triethylammonium bromide).

[0168] - Solvents: water and ethanol or isopropanol.

[0169] In each case, the amount of injected surface modifier was adjusted to have an acid molecule / zirconia molar ratio of 0.16, which corresponds to the TiO 2 Ti / ha or Ti / P of 6 in the example.

[0170] After this synthesis, the ZrO 2 Nanoparticles (naked or functionalized) were recovered as solutions in water and ethanol or isopropanol. They were centrifuged and washed 5 times with ethanol to remove unreacted surface mo...

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Abstract

The invention concerns a continuous flow process for manufacturing surface modified metal oxide nanoparticles by supercritical solvothermal synthesis in an reaction medium flowing within a continuous flow chamber, said continuous flow chamber containing a hydrolysis area and a supercritical area, said process comprising the introduction of a flow of metal oxide precursor into the continuous flow chamber at a point P located in the hydrolysis area or in the supercritical area, and the introduction of a flow of surface modifier into the continuous flow chamber at a point P2 located in the hydrolysis area or in the supercritical area, wherein P2 is located downstream of P1 with respect to the flow direction, as well as the device for carrying out this process.

Description

technical field [0001] The present invention relates to a continuous flow process for the manufacture of surface-modified metal oxide nanoparticles by supercritical solvothermal synthesis, and to an apparatus for carrying out this process. [0002] The method of the present invention can be used to make complex nanoparticles such as hybrid organic-inorganic nanoparticles that are readily available for the preparation of nanocomposites that can in turn be used in various fields such as optics, ceramics, catalysis, microelectronics , fuel cell technology, pharmaceuticals or cosmetics. Background technique [0003] Fine nanoparticles with narrow particle size distribution can be produced by various methods such as solid-state reaction, co-precipitation, sol-gel method, hydrothermal synthesis and solvothermal synthesis, plasma chemical vapor deposition or a combination of these methods. [0004] In nanotechnology, hydrothermal processing has advantages over other conventional m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053C01G25/02C01B13/36
CPCC01B13/366C01G23/053C01G25/02C01P2002/72C01P2002/82C01P2002/88C01P2004/04C01P2004/64C01B13/145Y02P20/54B01J3/006B01J3/008C09C1/043C09C1/24C09C1/3063C09C1/3669C09C1/407C09C3/08
Inventor M·泰奥德特C·爱莫尼尔
Owner ESSILOR INT CIE GEN DOPTIQUE
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