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Method for regulating and controlling particle size of silicon dioxide microspheres

A technology of silicon dioxide and microsphere particle size, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of complex reaction equipment, unfavorable promotion and application, poor economy, etc., and achieves easy operation, low experimental equipment requirements, and volatility. low effect

Pending Publication Date: 2018-11-23
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods are not conducive to widespread application due to complex reaction equipment, difficult operation, and poor economy.

Method used

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  • Method for regulating and controlling particle size of silicon dioxide microspheres
  • Method for regulating and controlling particle size of silicon dioxide microspheres
  • Method for regulating and controlling particle size of silicon dioxide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 0.1g of ammonium chloride in 20ml of deionized water, stir until completely dissolved, then add 20ml of 0.2mol / l ethyl orthosilicate, stir at 150r / min for 3h, dropwise add 1mol / L of triethylenetetramine solution , adjust pH=9, the solution becomes white and turbid, stop stirring, and let stand for 10h.

[0026] Then alternately washed three times with absolute ethanol and deionized water, dried in a vacuum drying oven at 60 °C for 4 hours, and finally placed the product in a muffle furnace at 550 °C for 6 hours, and the obtained silica microspheres had a diameter of about 400 nm. .

[0027] figure 1 A scanning electron micrograph of the silica microsphere powder in this example.

Embodiment 2

[0029] Dissolve 0.8g of ammonium chloride in 20ml of deionized water, stir until completely dissolved, then add 20ml of 0.2mol / l ethyl orthosilicate, stir at 150r / min for 3h, and dropwise add 1mol / L of triethylenetetramine solution , adjust pH=9, the solution becomes white and turbid, stop stirring, and let stand for 10h.

[0030] Then alternately washed three times with absolute ethanol and deionized water, dried in a vacuum drying oven at 60 °C for 5 hours, and finally placed the product in a muffle furnace at 550 °C for 6 hours, and the obtained silica microspheres had a diameter of about 1.2 μm. .

[0031] figure 2 A scanning electron micrograph of the silica microsphere powder in this example.

Embodiment 3

[0033] Dissolve 0.04g of ammonium chloride in 20ml of deionized water, stir until completely dissolved, then add 20ml of 0.2mol / l ethyl orthosilicate, stir at 150r / min for 3h, add 1mol / L triethylenetetramine solution dropwise, Adjust pH=9, the solution becomes white and turbid, stop stirring, and let stand for 10h.

[0034] Then alternately washed with absolute ethanol and deionized water for 3 times, dried in a vacuum drying oven at 60 °C for 4 h, and finally placed the product in a muffle furnace at 550 °C for 6 h. The diameter of the obtained silica microspheres was about 200 nm.

[0035] image 3 A scanning electron micrograph of the silica microsphere powder in this example.

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Abstract

The invention provides a method for regulating and controlling the particle size of silicon dioxide microspheres. The method comprises the following steps that an ammonium chloride aqueous solution and a tetraethoxysilane ethanol solution with different concentrations are mixed, the pH value of the solution is regulated and controlled through triethylene tetramine, at the normal-temperature and normal-pressure conditions, a submicron-order and micron-sized silicon dioxide sphere precursor with adjustable particle size is successfully synthesized, an obtained drying sample is placed in a mufflefurnace, calcining is carried out for 2-6 hours at the temperature of 500-800 DEG C, and cooling is carried out to reach the room temperature so as to obtain silicon dioxide with different sphericaldiameters. The regulation and control method has the advantages that a required device is simple, the operation is simple and easy, the efficiency is high, and accurate control over the size of the product can be realized; and the particle size of the silicon dioxide microspheres prepared through the method ranges from 200 nm to 2 microns, the synthetic path is simple, the cost is low, the application is wide, and the like.

Description

technical field [0001] The invention relates to a method for regulating the particle size of silica microspheres. Background technique [0002] Submicron silica microspheres have the characteristics of large specific surface area, strong adsorption, chemical stability, non-toxicity, and good biocompatibility, so they are widely used in advanced cosmetics, medicine, coatings, fillers and other fields. Has a wide range of applications. [0003] At present, the methods for preparing nano-submicron silica microspheres mainly include: vapor-phase precipitation method, sol-gel method and inverse microemulsion method. However, these methods are not conducive to wide popularization and application due to the complex reaction equipment, difficult operation, and poor economy. [0004] The publication number is CN103588210A The invention provides a preparation method of nano-silicon dioxide. The method is to add solution A (or solution B) into a percussion flow reactor, and use solut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/61C01P2004/62C01P2004/32C01P2004/03
Inventor 钟声亮李盛凯宁海金徐先进
Owner JIANGXI NORMAL UNIV
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