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Preparation method of nanometer silicon dioxide

A nano-silica, ammonium fluorosilicate technology, applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of low mixing efficiency, low added value, serious agglomeration and encapsulation, etc., to improve surface activity, Improve filtration strength and ensure integrity

Active Publication Date: 2012-06-20
WENGFU (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is simple in process, but due to the low mixing efficiency of the reactants in the conventional stirred reactor, the precipitation reaction cannot be uniformly and effectively controlled, and the product has quality problems such as coarse particles, wide particle size distribution, serious agglomeration and encapsulation, and cannot meet the requirements. High-end application requirements, low added value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 500 g of ammonium fluorosilicate solution with a concentration of 10% by mass, add 0.02 g of sodium lauryl sulfate, and adjust the speed of the mixer to 100 r / min; Add 487g of 10% ammonia water (110% of the theoretical amount), the addition rate of ammonia water is 24ml / min, the reaction temperature is controlled at room temperature, the reaction time is 60min, the aging time is 60min, and 0.1g of polypropylene with a mass percentage concentration of 1‰ is added Solution, stirring time 2min, wash the silica filter cake obtained by solid-liquid separation until neutral, dry the filter cake at 110°C, and perform calcination at 500°C to obtain a silica filter cake with a median particle size of 38nm. Silica powder.

Embodiment 2

[0016] Take 500 g of ammonium fluorosilicate solution with a concentration of 20% by mass, add 0.04 g of sodium lauryl sulfate, and adjust the speed of the mixer to 200 r / min; Pass 759.49g of 14% ammonia water (120% of the theoretical amount), the addition rate of ammonia water is 45ml / min, the reaction temperature is controlled at room temperature, the reaction time is 80min, the aging time is 70min, and 0.2g of polymer with a mass percentage concentration of 1‰ is added. Propylene solution, stirring time 4min, wash the silica filter cake obtained from solid-liquid separation until neutral, dry the filter cake at 120°C, and calcinate at 600°C to obtain a medium particle size of 43nm of silica powder.

Embodiment 3

[0018] Take 500 g of ammonium fluorosilicate solution with a concentration of 40% by mass, add 0.09 g of sodium lauryl sulfate, and adjust the speed of the mixer to 350 r / min; Pass through 1001.65g of 23% ammonia water (130% of theoretical amount), the addition rate of ammonia water is 85ml / min, the reaction temperature is controlled at room temperature, the reaction time is 80min, the aging time is 100min, and 0.3g of polymer with a mass percentage concentration of 1‰ is added. Propylene solution, stirring time 5min, wash the silica filter cake obtained from solid-liquid separation until neutral, dry the filter cake at 120°C, and calcinate at 620°C to obtain a medium particle size of 43nm of silica powder.

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Abstract

The invention discloses a preparation method of nanometer silicon dioxide, which comprises the following steps of: adding lauryl sodium sulfate into ammonium fluorosilicate solution as a surfactant; introducing ammonia solution and carrying out ammoniation reaction on the ammonium fluorosilicate solution, wherein the adding quantity of ammonia is 110-150 percent of theoretical amount; reacting at a normal temperature, strictly controlling the agitating speed, the adding speed of the ammonia and the reaction time, controlling the aging time within 60-150 min, adding polypropylene solution as a filter aid and carrying out solid-liquid separation after agitation; and calcining after the silicon dioxide is precipitated, washed and dried to obtain silicon dioxide powder with a median grain size of between 38-55 nm. The preparation method has the beneficial effects that as the ammonium fluorosilicate and the ammonia are taken as raw materials to prepare the nanometer silicon dioxide, and the lauryl sodium sulfate is taken as the surfactant, the surface activity of the silicon dioxide is improved; the reaction conditions are strictly controlled to prepare a silicon dioxide product with excellent performance; and the integrity of silicon dioxide powder crystals is ensured.

Description

technical field [0001] The invention relates to the field of preparation methods of inorganic chemical materials, in particular to a preparation method of nano silicon dioxide. Background technique [0002] Silica is commonly known as white carbon black, and its molecular formula is SiO 2 , Silica is insoluble in water and acids (except hydrofluoric acid), and aggregates into fine particles after absorbing water. It can dissolve in sodium hydroxide and hydrofluoric acid when heated, and is stable to other chemicals. Silica is high temperature resistant, non-combustible, and has good electrical insulation. [0003] The production methods of silica at home and abroad are mainly divided into gas phase method and precipitation method. The gas phase method is prepared by reacting silicon tetrachloride, oxygen (or air) and hydrogen as raw materials at high temperature. The quality of the product obtained by the gas phase method is good, but the preparation process is complicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y40/00
Inventor 杨三可解田李子燕隋岩峰刘松林杨丽萍冯胜波曾祥明骆吉林李白玉
Owner WENGFU (GRP) CO LTD
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