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Preparation method of modified nano silicon dioxide

A nano-silica, modification technology, applied in the treatment of dyed organic silicon compounds, fibrous fillers, etc., can solve the problems of large amount of modifiers, poor dispersion of organic compounds, long reaction time, etc., and reach the particle size distribution range Small size, prevention of secondary agglomeration, and high production efficiency

Active Publication Date: 2014-07-09
宿迁益创智能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, like other nanomaterials, nano-SiO 2 There are unsaturated residual bonds and hydroxyl groups in different bonding states on the surface, which makes nano-SiO 2 Particles have high surface activity and specific surface energy, are easy to agglomerate, and are poorly dispersed in organic compounds, which seriously affects the full play of various effects of nano-silica; for this reason, it is necessary to modify the surface of nano-silica to improve its performance. Application effect; at present, the existing technology for preparing modified nano-silica shows that SiO is prepared by sol-gel method 2 The in-situ modification technology of adding modifiers in the process is increasingly favored due to its advantages of simple process, uniform particles obtained, low energy consumption, low post-treatment pollution and high modification efficiency; sol-gel method to prepare modified nano The existing technology of silicon dioxide particles mainly uses a single substance as a catalyst, which has the problems of long reaction time and large amount of modifying agent; as disclosed in Chinese patent CN101880478A, a method for preparing hydrophobic nano-silica with controllable particle size , therefore, how to shorten the reaction time and increase the grafting rate of the modifier is of great significance to the research on the preparation of modified nanoparticles by sol-gel

Method used

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  • Preparation method of modified nano silicon dioxide
  • Preparation method of modified nano silicon dioxide
  • Preparation method of modified nano silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 4g of deionized water to 230g of ethanol, and oscillate ultrasonically for 10 minutes;

[0023] (2) Under ultrasonic vibration, add 10.4g tetraethyl orthosilicate (TEOS) into the above solution, and shake for 30 minutes;

[0024] (3) Use 0.1mol / L hydrochloric acid to adjust the pH value of the solution obtained in step (2) to 4, add 0.52g of silane coupling agent KH560 dropwise to the solution at a rate of 0.5g / min, and put the resulting system in Stir the reaction at a reaction temperature of 60°C for 6 hours;

[0025] (4) Adjust the pH value of the solution obtained in step (3) to 9 with 0.05mol / L ammonia water, and keep it warm for 2 hours;

[0026] (5) The modified nano-silica sol obtained in step (4) was dried, pulverized, sieved, washed with absolute ethanol for 5 times, washed with water, vacuum-dried at 80°C for 24 hours, and ground to obtain in-situ modified nano-silica sol. silica.

Embodiment 2

[0028] (1) Add 5g of deionized water to 230g of ethanol, and oscillate ultrasonically for 15 minutes;

[0029] (2) Under ultrasonic vibration, add 10.4g tetraethyl orthosilicate (TEOS) into the above solution, and shake for 30 minutes;

[0030] (3) Use 0.1mol / L hydrochloric acid to adjust the pH value of the solution obtained in step (2) to 3, add 1.04g of silane coupling agent KH560 to the solution dropwise at a rate of 0.5g / min, and put the resulting system in Stir the reaction at a reaction temperature of 60°C for 6 hours;

[0031] (4) Adjust the pH value of the solution obtained in step (3) to 9 with 0.05mol / L ammonia water, and keep it warm for 2 hours;

[0032] (5) The modified nano-silica sol obtained in step (4) was dried, pulverized, sieved, washed with absolute ethanol for 5 times, washed with water, vacuum-dried at 80°C for 24 hours, and ground to obtain in-situ modified nano-silica sol. silica.

Embodiment 3

[0034] (1) Add 7g of deionized water to 230g of ethanol, and ultrasonically shake for 10min;

[0035] (2) Under ultrasonic vibration, add 10.4g tetraethyl orthosilicate (TEOS) into the above solution, and shake for 30 minutes;

[0036] (3) Use 0.1mol / L hydrochloric acid to adjust the pH value of the solution obtained in step (2) to 5, add 1.56g of silane coupling agent KH560 dropwise to the solution at a rate of 0.5g / min, and put the resulting system in Stir the reaction at a reaction temperature of 60°C for 6 hours;

[0037] (4) Adjust the pH value of the solution obtained in step (3) to 9 with 0.05mol / L ammonia water, and keep it warm for 2 hours;

[0038] (5) The modified nano-silica sol obtained in step (4) was dried, pulverized, sieved, washed with absolute ethanol for 5 times, washed with water, vacuum-dried at 80°C for 24 hours, and ground to obtain in-situ modified nano-silica sol. silica.

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Abstract

The invention relates to a surface-modified nano silicon dioxide and a preparation method thereof, particularly a method for preparing lipophilic nano silicon dioxide by in-situ modification by a sol-gel process, belonging to the field of functional nano materials. The invention adopts a sol-gel process to prepare the nano silicon dioxide under the common catalytic action of acid and alkali, and performs in-situ modification on the nano silicon dioxide by using a silane coupling agent, so that the nano silicon dioxide becomes lipophilic instead of hydrophilic. The wetting property and dispersity of the modified nano silicon dioxide in the polymer are improved.

Description

technical field [0001] The invention relates to a surface-modified nano-silica and a preparation method thereof, in particular to a method for preparing lipophilic nano-silica by in-situ modification using a sol-gel method, and belongs to the field of functional nanometer materials. Background technique [0002] In recent years, polymer / inorganic nanocomposites have attracted widespread attention and achieved rapid development due to their unique properties. The excellent properties of the particles, such as strength, modulus, and dimensional stability, also provide the possibility to endow the material with new special functions. Nano-silica is an amorphous, non-toxic, odorless, and non-polluting white powder non-metallic material , is one of the earliest nanomaterials, and it is also a nanopowder material produced on a large scale in the world. As an excellent structural and functional material, nanosilica has high surface activity, high specific surface area, and low spec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/28C09C3/12
Inventor 宋仁国姜冬王超李鑫伟
Owner 宿迁益创智能科技有限公司
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