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A kind of method that utilizes gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol

A slurry reactor, gas-liquid-solid technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve problems such as the dispersibility of silicon powder and silica sol particles that are not involved, and achieve the effect of uniformity

Active Publication Date: 2018-10-12
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, both of the above are to achieve the purpose of controlling particle size and particle size distribution by controlling the dynamic factors of silicon powder hydrolysis and particle growth, and do not involve the description of the dispersion of silicon powder and silica sol particles in the system.

Method used

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  • A kind of method that utilizes gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol
  • A kind of method that utilizes gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol
  • A kind of method that utilizes gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol

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Experimental program
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Embodiment 1

[0024] A kind of method utilizing gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol, its component counts in parts by mass, comprises the following process steps:

[0025] The length-to-diameter ratio of the gas-liquid-solid three-phase slurry reactor is 50:1; the silicon powder particle size is 100 mesh, and the addition amount is 7 parts, which are added in 3 times with an interval of 20 minutes each time; It is composed of 99.95 parts of water, and the liquid feeding rate is 0.5mL / min; the mass ratio of silicon powder and alkali is 10:1; the reaction temperature is 50°C, and the reaction is kept for 2 hours after stopping the feeding of alkali solution. The obtained silica sol has a particle size of 13 nm and a polydispersity index of 0.021. figure 2 It is the particle size distribution diagram of the silica sol obtained under the present embodiment.

Embodiment 2

[0027] A kind of method utilizing gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol, its component counts in parts by mass, comprises the following process steps:

[0028] The length-to-diameter ratio of the gas-liquid-solid three-phase slurry reactor is 250:1; the particle size of silicon powder is 200 mesh, and the addition amount is 50 parts, which is added in 4 times with an interval of 120 minutes; It is composed of 99 parts of water, and the liquid feeding rate is 5mL / min; the mass ratio of silicon powder and alkali is 20:1; the reaction temperature is 70°C, and the reaction is kept for 10 hours after stopping the feeding of alkali solution. The obtained silica sol has a particle size of 20 nm and a polydispersity index of 0.012. image 3 It is the scanning electron micrograph of the silica sol obtained under the present embodiment.

Embodiment 3

[0030] A kind of method utilizing gas-liquid-solid three-phase slurry reactor to prepare monodisperse silica sol, its component counts in parts by mass, comprises the following process steps:

[0031] The length-to-diameter ratio of the gas-liquid-solid three-phase slurry reactor is 100:1; the particle size of silicon powder is 600 mesh, and the addition amount is 100 parts, which is added in 6 times with an interval of 80 minutes each time; , 1 part KOH, 0.5 part NH 4 Composed of OH and 97.5 parts of water, the liquid feed rate is 2mL / min; the mass ratio of silicon powder and alkali is 50:1; the reaction temperature is 90°C, and the reaction is kept for 12 hours after stopping the feeding of alkali solution. The obtained silica sol has a particle size of 50 nm and a polydispersity index of 0.036. Figure 4 It is the scanning electron micrograph of the silica sol obtained under the present embodiment.

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Abstract

The invention discloses a method for preparing monodisperse silica sol by utilizing a gas-liquid-solid three-phase slurry reactor. The method is characterized by comprising the following step: adding alkali liquor and silica powder into the slurry reactor, wherein the alkali liquor is continuously added, and the silica powder is added in batches. According to the invention, based on the mechanism of free ascend of gas in a liquid phase on agitation action of the system, a good stirring effect is achieved by utilizing the characteristics of gas (H2) produced by silica powder hydrolysis, such as small volume, dispersion uniformity and uniform size, so that the silica powder is in a suspended state in the reactor and is fully contacted with the liquid phase. An extra bubbling device is not needed in the reactor, and the stirring requirement needed by the reaction can be met. The obtained silica sol has the advantages of regular morphology, uniform particle size and monodisperse property.

Description

technical field [0001] The invention relates to a method for preparing silica sol, in particular to a method for preparing monodisperse silica sol by using a gas-liquid-solid three-phase slurry reactor. Background technique [0002] Silica sol refers to the dispersion system of amorphous silicon dioxide in water or other solvents, which has the properties of colloid and has a particle size of 5-100nm. Due to its huge specific surface area and peculiar surface characteristics of particles, it is widely used in chemical mechanical polishing (CMP), electronics industry, industrial catalysis, textile, papermaking and other fields. Especially the application of large particle size and monodisperse silica sol is favored. Generally, the definition of large particle size is that the particle size is larger than 20nm. [0003] At present, the methods for preparing silica sol mainly include silica powder hydrolysis method, ion exchange method, sol-gel method, sodium silicate acidifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/141
Inventor 张春芳周波白云翔孙余凭顾瑾
Owner JIANGNAN UNIV
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