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Method for preparing high-purity mono-disperse silicon dioxide hydrosol

A silicon dioxide, monodisperse technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve problems such as inconvenience in work, introduction of metal impurities, and restrictions on the localization of HPLC chromatographic packing, so as to improve catalytic activity and accelerate Reaction process, the effect of ensuring high purity

Inactive Publication Date: 2011-02-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the silica sols that have been disclosed for preparing porous spherical silica gel for chromatography mostly use sodium hydroxide and ammonia water or water glass as catalysts, which will inevitably introduce metal impurities into the system, causing great damage to subsequent work. inconvenient
[0008] Since domestically produced commercial silica hydrosol is difficult to achieve high purity and monodisperse, it is correspondingly difficult to prepare high-purity spherical, monodisperse porous silica gel, which restricts the further localization of industries such as HPLC chromatographic packing.

Method used

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  • Method for preparing high-purity mono-disperse silicon dioxide hydrosol
  • Method for preparing high-purity mono-disperse silicon dioxide hydrosol

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In the 500ml there-necked flask equipped with a reflux device, add 180ml concentration of 25%-28% analytical pure ammonia water, turn on the water bath and heat up to 50°C, turn on the stirring, set the stirrer speed to 400rpm, add the silicon powder (99.99 %, 200 mesh) about 16.0g (±0.1g), continue to heat up. Wait until the temperature of the water bath reaches 80°C and keep warm, then add 50ml of ammonia water to the reaction vessel at the rate of 10ml drops for half an hour. After keeping warm for about 2 hours, start to feed ammonia gas intermittently, and keep the pH value of the reaction solution not less than 11, and finish the reaction after 4 hours. The obtained silica hydrosol was filtered to remove unreacted silica powder.

[0022] Take three 20ml beakers, label and weigh them respectively. Weigh 2.00g (±0.02g) of the filtered silicon hydrosol into three beakers, weigh the beakers, put them in an oven and dry them at 70°C. Take out the beakers after dryin...

Embodiment 2

[0025]In the 500ml there-necked flask equipped with a reflux device, add 160ml concentration of 25%-28% analytical pure ammonia water, turn on the water bath and heat up to 50°C, turn on the stirring, set the speed of the stirrer to 600rpm, add the silicon powder weighed in advance (99.99 %, 200 mesh) about 16.0g (±0.1g), continue to heat up. Keep warm until the water bath temperature reaches 80°C, then add 40ml of ammonia water to the reaction vessel at the rate of 20ml drops for 1 hour. After keeping warm for about 2 hours, start to feed ammonia gas intermittently, and keep the pH value of the reaction solution not less than 11, and finish the reaction after 4 hours. The obtained silica hydrosol was filtered to remove unreacted silica powder.

[0026] Take three 20ml beakers, label and weigh them respectively. Weigh 2.00g (±0.02g) of the filtered silica sol into three beakers, weigh the beakers and place them in an oven to dry at 70°C. Take out the beakers after drying, w...

Embodiment 3

[0028] In the 500ml there-necked bottle equipped with a reflux device, add 200ml concentration of 25%-28% analytically pure ammonia water, turn on the water bath and heat up to 50°C, turn on the stirring, set the stirrer speed to 600rpm, add the silicon powder (99.99 %, 200 mesh) about 16.0g (±0.1g), continue to heat up. Wait until the temperature of the water bath reaches 80°C and keep warm, then add 60ml of ammonia water to the reaction vessel at the rate of 10ml drops for half an hour. After keeping warm for about 2 hours, start to feed ammonia gas intermittently, and keep the pH value of the reaction solution not less than 11, and finish the reaction after 4 hours. The obtained silica hydrosol was filtered to remove unreacted silica powder.

[0029] Take three 20ml beakers, label and weigh them respectively. Weigh 2.00g (±0.02g) of the filtered silicon hydrosol into three beakers, weigh the beakers, put them in an oven and dry them at 70°C. Take out the beakers after dr...

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Abstract

The invention discloses a method for preparing high-purity mono-disperse silicon dioxide hydrosol. The method comprises the following steps: a hydrolysis reaction is performed on monocrystal silicon powder serving as a silicon source by taking ammonia as a catalyst, the reaction is performed in a heating, stirring and ammonia (99.99 percent) atmosphere; the reactive liquid is filtered after the reaction is completed to obtain the high-purity mono-disperse silicon dioxide hydrosol product. In the silicon dioxide hydrosol prepared by adopting the method, the solid content is between 20 and 35 percent, and the sphere particle size distribution is between 25 and 35nm. In the preparation process, high-purity silicon powder is used as a silicon source instead of sodium silicate and other soluble silicate or orthosilicate, ammonia is used as the catalyst instead of alkaline metal, so metal impurities (such as sodium, iron, aluminum and the like) introduction or residual ester and alcohol is effectively avoided, and high purity of the product is ensured. The product has great potential application value in self assembly of photonic crystal, chromatography packing, size reference material, planar display and other fields.

Description

technical field [0001] The invention relates to a method for manufacturing non-toxic, tasteless and non-polluting ultrafine inorganic materials, in particular to a method for preparing high-purity, monodisperse silicon dioxide hydrosol. Background technique [0002] Silica sol, also known as colloidal silica (Colloidal Silica), is a white or slightly blue opalescent colloidal solution. Since its main component is hydrated silica in colloidal form, its molecular formula can be expressed as mSiO 2 ·nH 2 O. [0003] Monodisperse SiO 2 It is a kind of spherical particles with very uniform size, and the particle size that can be selected ranges from tens of nanometers to several microns. It can be porous or non-porous. After surface bonding or coating other organic or inorganic materials, it can be endowed with specific chemical activity or physical properties such as light, electricity, and magnetism, and because nano-SiO 2 The quantum size effect and macroscopic quantum tun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/141
Inventor 杨俊佼张硕
Owner BEIJING UNIV OF CHEM TECH
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