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Method for preparing nano-silica with controllable particle size

A nano-silica, particle size technology, applied in the field of nano-silica preparation, can solve the problems of low purity, large particle radius, etc.

Inactive Publication Date: 2014-04-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(3) Precipitation method: its characteristics are simple and easy to implement, but the purity is low and the particle radius is large; therefore, based on improving the purity of nanoparticles and according to the different needs of different industries for the particle size of nano-silica, there is an urgent need for a particle size Controlled Silica Production Process

Method used

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  • Method for preparing nano-silica with controllable particle size
  • Method for preparing nano-silica with controllable particle size
  • Method for preparing nano-silica with controllable particle size

Examples

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preparation example Construction

[0024] Preparation of PAMAM template

[0025] 1. Preparation of 0.5-generation PAMAM: Put 120g of methyl acrylate and 10g of methanol in a 400mL volumetric flask, stir magnetically at 5°C, pass He protection for 1h, and add 10.5g of ethylenediamine and 27.5g of methanol with a dropping funnel. The mixture was added dropwise for 1h and passed through He. After the addition, the reaction was carried out at room temperature for 36h. Use a rotary evaporator to distill under reduced pressure (approximately 140Pa, 40°C) to remove unreacted methyl acrylate and methanol to obtain a slightly yellow and slightly viscous liquid.

[0026] 2. Preparation of 1.0-generation PAMAM: Put 84g of ethylenediamine and 11g of methanol in a 500mL volumetric flask, stir magnetically at 5°C, pass He protection for 1h, and add 20g of 0.5-generation PAMAM and 64g of methanol with a dropping funnel. The mixture was added dropwise for 2h and passed through He. After the addition was completed, reacted for 36h ...

Embodiment 1

[0036] Example 1: Using 6.0 generation PAMAM as a template to prepare nano-silica, its primary particle size is between 500-650nm and the specific surface area is 11.8-6.9m 2 / g.

[0037] Preparation of nano-particle silica

[0038] Nano SiO 2 The main steps of the preparation:

[0039] 1. Put 100g of the prepared 6.0-generation PAMAM into a 350g mixed solvent of water and methanol, and dissolve it in a closed container (the ratio of water to methanol is 1:3, and the water should be heated at 35℃) , The dissolution time is 30min, use analytically pure ammonia and dilute hydrochloric acid to adjust the pH value to 8-9, as the base fluid for use.

[0040] 2. Add 150g of 28% potassium water glass to the mixed base solution at a rate of 150 drops per minute, and use dilute hydrochloric acid to adjust the pH of the solution at 6~7. Stir and add for 0.5 hours. After that, keep stirring for 1h;

[0041] 3. Filter the resulting precipitate, wash it with a mixed solvent of water and methanol (...

Embodiment 2

[0045] Example 2: The steps for preparing nano-silica with 4.0-generation PAMAM as a template are the same as above. Its primary particle size is between 560~770nm, and the specific surface area is between 10.2~5.3m 2 / g, SiO prepared 2 High purity, uniform particle size distribution, single particle size, no hard agglomeration, and extremely high practical value.

[0046] 1. Prepare the prepared 4.0 generation PAMAM (for molecular structure, please refer to figure 1 ) 100g, put it into 350g of mixed solvent of water and methanol, and dissolve in a closed container (the ratio of water to methanol is 1:3, and the water should be hot water at 35℃), the dissolution time is 30min, use analysis Adjust the pH value to 8-9 with pure ammonia water and dilute hydrochloric acid, and use it as a base liquid.

[0047] 2. Add 150g of 28% potassium water glass to the mixed base solution at a rate of 150 drops per minute, and use dilute hydrochloric acid to adjust the pH of the solution at 6~7. S...

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Abstract

A method for preparing nano-silica with a controllable particle size belongs to the technical field of preparation of silica nano-particles. The method comprises dissolving 4.0 to 6.0 generation of PAMAN in a mixed solvent of methanol and water in a ration of 1 : 3, and adjusting a pH value of the solution to 8 to 9 by using acid and / or ammoniacal liquor and using the solution as a base solution; adding dropwisely sodium silicate solution with a mass concentration of 20% to 35% into the base solution with stirring and adjusting the pH to weak acidity in the range of 6 to 7; and filtering, washing, drying at a low temperature 0 DEG C and grinding generated precipitates. The mass ratio of the PAMAN to the mixed solvent of methanol and water to the sodium silicate solution is (98 to 102) : 350 : (140 to 160). The prepared sillica has advantages of high purity, uniformly distributed and single particle size and no hard agglomeration, and has extremely high practical value.

Description

Technical field [0001] The invention belongs to the technical field of the preparation of silica nanoparticles, and in particular relates to a method for preparing nano silica with a controllable particle size. Background technique [0002] Nano-silica is an amorphous white powder, a non-toxic, odorless, and non-polluting non-metallic material. The particle structure is very special. There are unsaturated residual bonds and hydroxyl groups in different bonding states on the surface of the particles. Its molecular state is a three-dimensional chain structure. This special structure gives it unique properties: such as reflectance of ultraviolet rays within a wavelength of 49nm. As high as 70% to 80%; when nano-silica is combined with polymer materials, it can improve the thermal, light and chemical stability of polymer materials, and improve the aging resistance and chemical resistance of products; it can achieve UV aging resistance And the purpose of heat aging; it can improve th...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y40/00
Inventor 靳涛李效玉
Owner BEIJING UNIV OF CHEM TECH
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