Preparation of mineral particles in a supercritical CO2 medium

A kind of inorganic particles, supercritical technology, applied in the process of supercritical conditions, inorganic chemistry, liquid into beads and granulation, etc., can solve the problems of high internal porosity, reduce process costs, reduce liquid and The effect of gas effluent

Inactive Publication Date: 2010-06-23
FRAMATOME ANP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the particles obtained according to this type of process, a high internal porosity is generated, which leads to the formation of cavities, which are more pronounced the larger the particles formed

Method used

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  • Preparation of mineral particles in a supercritical CO2 medium
  • Preparation of mineral particles in a supercritical CO2 medium
  • Preparation of mineral particles in a supercritical CO2 medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0097] ZrO 2 Synthesis of particles (unsintered)

[0098] In this example, ZrO was synthesized by the method of the present invention from a medium (F1) prepared under the following conditions 2 Granules:

[0099] - 1.5 g zirconium ethoxide (i.e. 5.5 x 10 -3 mol) reflux heated to 50 ° C for 3 hours,

[0100] -Join 5.5×10 -3 mol formic acid, the medium was then heated to reflux again to 50°C for 30 minutes,

[0101] -Then add 0.54g HNO to the obtained medium 3 70% aqueous solution.

[0102] The medium (F1) obtained after the above-mentioned steps is in liquid form and has a milky appearance.

[0103] The medium (F1) was placed in a container 15 and injected through the injection nozzle 10 at a rate of 20 ml / hour at a pulse rate of two drops per second (pulse valve) under the following conditions:

[0104] - temperature in the injection chamber 20: 200°C;

[0105] - temperature in the recovery chamber 40: 315 °C;

[0106] - an increasing temperature gradient between th...

Embodiment 2

[0111] ZrO introduced into preformed SiC particles 2 Synthesis of particles

[0112] In this example, particles were synthesized by the method of the invention from a medium (F2) prepared under the following conditions:

[0113] -While stirring will contain 3g of zirconium ethoxide (i.e. 11×10 -3 mol), 20g ethanol and 0.54g70% HNO 3 The mixture of aqueous solutions is heated to reflux to 50° C. for 4 hours, thereby dissolving the zirconium ethoxide in the medium;

[0114] -The medium is then allowed to cool to ambient temperature (25° C.) and 4 g of water and 5.5×10 -3 mol formic acid, the medium was stirred for 1 hour;

[0115] - Add 0.019 g of SiC crystals with an average diameter of 30 nm to the medium.

[0116] The medium (F2) obtained after the above-mentioned steps is in the form of a polymer gel whose fluid properties depend on the time and speed of stirring (thixotropic effect).

[0117] This medium (F2) was placed in a container 15 and injected through the injec...

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Abstract

The invention relates to a method for preparing mineral particles (p) from mineral particle precursors, said method comprising a step (E) that comprises injecting a fluid medium (F) containing said precursors in solution and/or dispersed in a solvent in a reactor containing CO2 at a supercritical state using an injection nozzle giving into an area where the supercritical CO2 is at a temperature higher than or equal to the conversion temperature of the precursors into corresponding mineral species, the invention also relates to particles (p) obtained according to the method and to the use thereof.

Description

technical field [0001] The present invention relates to a process for obtaining inorganic particles of millimeter size, which particles also have high compactness and a large specific surface area. These easy-to-handle and non-powder-like particles are especially suitable for the preparation of ceramic materials and / or catalysts, especially metal catalysts. Background technique [0002] Many methods of preparing inorganic particles for forming ceramic materials and catalysts are currently known. [0003] Within this range, some processes employ sol / gel type methods. Such methods are advantageously carried out in a supercritical fluid medium rather than a liquid medium, which avoids the use of especially large quantities of solvents (and their work-up which can prove to be problematic), and also makes it possible to dispense with the use of The obtained granules are washed and dried. However, processes using sol / gel-type methods in supercritical fluid media generally resul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J3/00C01B33/18C01G25/02B01J35/08C01G43/025C01G56/00C04B35/622C04B35/482G21C3/62B01J19/26
CPCC04B2235/5409B01J2219/185B01J2219/00119C04B2235/441B01J2/02C04B35/62823C04B35/486C04B2235/5454C04B2235/449B01J19/26B01J2208/00672B01J2219/00173B01J21/066B82Y30/00C04B35/62655B01J35/08C01G43/01C01B33/18C01G25/02C01G23/047C01G9/02B01J4/002C01P2006/12B01J3/008C04B2235/3826C01G56/00C04B2235/528C04B2235/5427C01P2004/02C01G27/02Y10T428/2982Y02P20/54
Inventor B·萨拉S·维勒曼J·马祖瓦耶T·穆勒N·马斯吉雷兹D·科特A·朱贝P·吉耶米耶
Owner FRAMATOME ANP
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