Preparation method of micron spherical silicon oxide

A technology of spherical silica and silica powder, which is applied in the chemical industry, can solve problems such as poor density, high energy consumption, and serious agglomeration, and achieve the effects of high mechanical strength and high water absorption of the carrier

Active Publication Date: 2018-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN104192853A is to mix tert-butanol and ethylenediamine with water glass, then add sulfuric acid into water glass, a chemical precipitation reaction occurs, and spherical silica is obtained. The main disadvantage is that the particle size distribution is not easy to control and restricts the comparison of molding conditions. Many, and the phenomenon of reunion is serious
Patent CN102249248A is prepared by using tetraethyl orthosilicate as the silicon source, alcohol as the co-solvent, and hydrolysis and condensation under alkaline conditions. The prepared silica particles have micropores, poor density, looseness, and easy pulverization; the patent CN101708854A sprays instant potassium silicate solid particles into inorganic acid through high-pressure gas, controls the injection cycle time to obtain the mixture and then separates the product. It is a combination of microemulsion and spray method in disguise. Although the process is simple, the particle strength of the product obtained is Poor, pore volume and pore diameter are uncontrollable; CN101462727 burns natural gas and oxygen, melts it with a high-temperature flame to form silica, and makes it spheroidize by the surface tension after melting, and then large flow of pure oxygen and natural gas will make the silica The particles are effectively blocked and dispersed, the pore size and pore volume of the obtained particles are uncontrollable, the particle size is uneven, there is agglomeration phenomenon, the operating conditions are harsh, and the energy consumption is high.

Method used

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  • Preparation method of micron spherical silicon oxide
  • Preparation method of micron spherical silicon oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1-1) Weigh an average of 100 mesh SiO 2 21g of powder, 15ml of concentrated hydrochloric acid, 126g of 30%wt alkaline silica sol (wherein the average particle size of silicon oxide is 25nm) and 10ml of methanol are fully mixed to obtain a slurry, and then 15g of hexamethylenetetramine is added to the slurry, fully dissolve.

[0029] (1-2) Select a nozzle with an aperture of 0.25mm and install it on the jet generator, inject the slurry obtained in (1-1) into 25# transformer oil at 95°C at a speed of 5m / s, and let it stand for aging for 4 After hours, the shaped pellets were separated from the oil and dried under vacuum at 80°C for 12 hours.

[0030] (1-3) The obtained product was washed until neutral, then dried at 140°C for 10 hours, and calcined at 550°C for 12 hours to obtain micron spherical silicon oxide particles.

[0031] After characterization, the BET specific surface area of ​​Example 1 is 394.1m 2 / g, the pore volume is 0.949cm 3 / g, the average pore diam...

Embodiment 2

[0033] (2-1) Weigh an average of 100 mesh SiO 2 21g of powder, 5ml of concentrated nitric acid, 126g of 30%wt alkaline silica sol (the average particle size of silicon oxide is 25nm) and 10ml of ethanol are fully mixed to obtain a slurry, and then 2g of wollastonite (300 mesh) and hexamethylene Tetramine 15g is added in the slurry, fully dissolved.

[0034] (2-2) Select a nozzle with an aperture of 0.25mm and install it on the jet generator, inject the slurry obtained in (2-1) into 25# transformer oil at 90°C at a speed of 5m / s, and separate it from the oil The formed pellets were vacuum-dried at 60° C. for 24 hours.

[0035] (2-3) The obtained product was washed until neutral, then dried at 140°C for 10 hours, and calcined at 550°C for 12 hours to obtain micron spherical silicon oxide particles.

[0036] After characterization, the BET specific surface area of ​​embodiment 2 is 393.5m 2 / g, the pore volume is 0.993cm 3 / g, the average pore diameter is 9.726nm, and the bul...

Embodiment 3

[0038] (3-1) Weigh an average of 100 mesh SiO 2 31g of powder, 10ml of concentrated phosphoric acid, 126g of 30%wt alkaline silica sol (the average particle size of silicon oxide is 25nm) and 8ml of polyethylene glycol are fully mixed to obtain a mixed slurry, and then 2.5g of silicon carbide fiber (500 mesh) and hexamethylenetetramine 14g are added in the slurry, fully dissolved.

[0039] (3-2) Select a nozzle with an aperture of 0.35mm and install it on the jet generator, inject the slurry obtained in (3-1) into 25# transformer oil at 90°C at a speed of 5m / s, and form it from the oil The formed pellets were isolated and dried under vacuum at 80°C for 16 hours.

[0040] (3-3) The obtained product was washed until neutral, then dried at 140°C for 10 hours, and calcined at 550°C for 12 hours to obtain micron spherical silicon oxide particles.

[0041] After characterization, the BET specific surface area of ​​embodiment 3 is 400.6m 2 / g, the pore volume is 0.987cm 3 / g, the...

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Abstract

The invention discloses a preparation method of micron spherical silicon oxide. The method mainly comprises the following steps: pre-mixing silicon oxide powder and colloidal silica solution, adding acid, an additive, a dispersing agent and organic amine, sufficiently mixing the materials to form slurry, injecting the slurry into an oil column for molding through a fluidic generator with a certainaperture, and conducting aging, washing, drying and roasting to obtain the micron spherical silicon oxide particles. The micron spherical silicon oxide particles obtained by the method of the invention have mesoporous characteristics, aperture size controllable within 2-50 nm, specific surface area of 200-450 m<2>/g, pore volume of 0.5-1.5 ml/g, and grain size of 1-500 [mu]m. The micron sphericalsilicon oxide prepared by the method of the invention can be applied to the fields such as heterogeneous catalytic reaction, absorptive separation materials and liquid chromatographic fillers.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of micron spherical silicon oxide. Background technique [0002] Silicon oxide is an attractive research object in the field of nanomaterials and chemical industry in recent years. It is one of the porous solid substances. Silicon oxide has a large specific surface area and uniform pore size, and plays an important role in the field of catalysis and separation, especially in the fields of catalysis, separation and purification, drug embedding and slow release, gas sensing and so on. According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), those with a pore diameter less than 2 nanometers are called micropores; those with a pore diameter larger than 50 nanometers are called macropores; hole). Since the pores have an important influence on the diffusion of substances, the mesoporous silica is of great...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/32C01P2004/61C01P2006/12C01P2006/14C01P2006/16C01P2006/17
Inventor 苏宏久杨晓野王树东李大卫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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