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Sol-solvent-thermal method for synthesizing nanocrystalline oxide powder

A technology of oxide powder and nanocrystals, which is applied in chemical instruments and methods, titanium oxide/hydroxide, oxide/hydroxide preparation, etc., to achieve the effects of controllable size, low raw material cost, and good crystal shape development

Inactive Publication Date: 2009-01-21
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the invention is to prevent the agglomeration of nanoparticles and realize the low-temperature synthesis of monodisperse nanocrystalline powders. For this reason, a new method of sol-solvothermal is provided, which overcomes the expensive raw materials used in traditional sol-gel methods ( alkoxide), which overcomes the deficiency that the high temperature hydrolysis of the hydrothermal method is easy to produce agglomeration

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  • Sol-solvent-thermal method for synthesizing nanocrystalline oxide powder
  • Sol-solvent-thermal method for synthesizing nanocrystalline oxide powder
  • Sol-solvent-thermal method for synthesizing nanocrystalline oxide powder

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preparation example Construction

[0030] (3) Preparation of sol (sol): at a certain temperature, under stirring, the prepared reactant solution is slowly added dropwise to the prepared inorganic salt mother liquor, and after the addition is completed, the reaction is continued for a period of time to obtain a transparent Sol;

[0031] (4) Solvothermal reaction of the sol: the prepared sol is placed in a reaction kettle, reacted at a certain temperature and pressure for a suitable time, and the formed product is filtered, washed and dried to obtain a nanocrystalline oxide powder.

Embodiment 1

[0033] Weigh 3.113g TiCl 4 , carefully added to 50mL of ethanol at 0°C, and then 50mL of ethylene glycol, and stirred thoroughly to obtain a 0.164mol / L titanium salt mother liquor. Weigh 2.725g of concentrated ammonia water (wt%=25-28%, the same below) and 0.5g of polyvinylpyrrolidone (PVP), and sequentially add them into 30mL of ethanol to prepare a 1.4mol / L precipitation reagent solution. Place the mother liquor in a constant temperature water bath at 80°C and stir it fully; after preheating for 5 minutes, slowly drop the precipitation reagent solution into the mother liquor at a rate of about 1 mL / min; after the precipitation reagent solution is added dropwise, continue to The temperature was reacted for 30 min, and finally a clear and transparent colorless sol was obtained. Measure 40mL of sol, put it in a self-pressurized reactor with a volume of 50mL, and react at a temperature of 150°C, a pressure of 1MPa, and a time of 3h. After the reaction, the reaction kettle was ...

Embodiment 2

[0035] Weigh 2.0g FeCl 3 ·6H 2 O, join in 50mL ethanol, add 50mL glycerol again, and fully stir, obtain the iron salt mother liquor of 0.074mol / L. Weigh 0.970g of concentrated ammonia water and 0.2g of polyvinylpyrrolidone (PVP), and add them to 30mL of ethanol in sequence to prepare a 0.5mol / L precipitant solution. Place the mother liquor in a constant temperature water bath at 80°C and stir it fully; after preheating for 5 minutes, slowly drop the precipitation reagent solution into the mother liquor at a rate of about 1 mL / min; after the precipitation reagent solution is added dropwise, continue to The temperature was reacted for 30 min, and finally a clear and transparent brown-yellow sol was obtained. Measure 40mL of sol, put it in a self-pressurized reactor with a volume of 50mL, and react at a temperature of 150°C, a pressure of 1MPa, and a time of 3h. After the reaction, the reaction kettle was naturally cooled to room temperature, and the slurry was taken out, cent...

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Abstract

The invention provides a sol-solvent thermal method for synthesizing a nanocrystalline oxide powder. The method comprises the following: (1) a step of preparation of inorganic salt mother liquids, during which the inorganic salt taken as a material is dissolved in an organic liquid medium or water to prepare a mother liquid of the inorganic salt with definite concentration; (2) a step of preparation of a precipitation reactant liquid, during which alkali is dissolved in an organic liquid medium or water, proper quantity of surfactants are added to prepare the precipitation reactant liquid with definite concentration; (3) a step of preparation of sols, during which, at a certain temperature, while stirring, the prepared reactant liquid is slowly added in the prepared mother liquid of the inorganic salt, the reactant liquid and the mother liquid of the inorganic salt are kept reacting for a period of time after adding the reactant liquids in the mother liquid of the inorganic salt, and the transparent sols are obtained; and (4) a step of solvent thermal reaction of the sols, during which the prepared sols are put in a reaction kettle and reacted for a period of time under a certain temperature and pressure, the products obtained are subjected to filtering, washing and drying, and the nanocrystalline oxide powder is obtained.

Description

technical field [0001] The invention relates to a preparation technology of inorganic non-metallic material nano powder, in particular to a synthesis technology of preparing oxide nano crystal by sol-solvothermal method. Background technique [0002] Nano-oxides are widely used in the production of catalysts, fine ceramics, composite materials, magnetic materials, fluorescent materials, moisture-sensitive sensors, and infrared-absorbing materials. The preparation of nano-metal oxides can generally be divided into gas-phase method, liquid-phase method and solid-phase method. Compared with the gas-phase method and the solid-phase method, the liquid-phase method is easier to control the nucleation-growth, and it is easier to control the chemical composition of the particles. For materials with complex compositions, powders with good chemical uniformity can also be obtained. The liquid phase method is divided into solvent-gel method, precipitation method, hydrolysis method, hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01F17/00C01G23/053C01G49/02C01F7/02C01G9/02C01G25/02
Inventor 卢旭晨姚生永
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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