A kind of hydrophilic silicon dioxide airgel microsphere and preparation method thereof

A technology of hydrophilic silica and silica, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve problems such as industrial production limitations and complicated purification process, and achieve strong pressure bearing capacity and mechanical strength High, simple post-processing effects

Active Publication Date: 2019-05-03
上海特栎材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because it involves the use of a large amount of surfactants and non-polar organic solvents, the later purification process is complicated, and industrial production is still limited

Method used

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  • A kind of hydrophilic silicon dioxide airgel microsphere and preparation method thereof
  • A kind of hydrophilic silicon dioxide airgel microsphere and preparation method thereof
  • A kind of hydrophilic silicon dioxide airgel microsphere and preparation method thereof

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preparation example Construction

[0034] The invention provides a method for preparing hydrophilic silica airgel microspheres, comprising the following steps:

[0035]1) Synthesis of siloxane prepolymer: Stir tetraalkoxysilane, hydroxyl-containing hydrophilic compound and the first solvent at a speed of 100-1000 rpm until transparent, add dilute acid solution, after the reaction is complete, remove Solvent, obtain siloxane prepolymer; The concentration C of described dilute acid solution H+ =1-6mol / L; the weight ratio of the dilute acid to tetraalkoxysilane is 0.01-0.2:1;

[0036] The first solvent is alcohol, ether or ketone; the hydrophilic compound containing hydroxyl is polyalcohol, monosaccharide or polysaccharide;

[0037] In this step, the alkoxy group of the tetraalkoxysilane is one or more of methoxy, ethoxy and isopropoxy. The hydroxyl-containing hydrophilic compound can be polyethylene glycol with an average molecular weight of 200-10000, polyvinyl alcohol with an average molecular weight of 200-1...

Embodiment 1

[0043] A preparation method for hydrophilic silicon dioxide airgel microspheres, comprising the following steps:

[0044] (1) Mix 278.32 grams of tetraethyl orthosilicate, 150 grams of ethanol, and 10 grams of polyethylene glycol (average molecular weight 1000) until transparent; 15 grams of concentrated hydrochloric acid (mass concentration is 37%) and 20 grams of water are mixed evenly , and then drop it slowly, after the addition is completed, heat up to 60 degrees, continue to stir for 2 hours, and quickly distill off the ethanol in the system under reduced pressure to obtain a fluid, transparent silicone prepolymer with a certain viscosity ;

[0045] (2) Add 50 grams of the above-mentioned siloxane prepolymer to 100 grams of distilled water under high-speed stirring (500 rpm), and after the addition is completed, adjust the pH to 10 with ammonia water, and continue stirring for 2 hours to obtain a white emulsion ;

[0046] (3) Let the above emulsion stand for 1 hour to ...

Embodiment 2

[0049] The difference between embodiment 2 and embodiment 1 is that tetraethyl orthosilicate is replaced by tetramethyl orthosilicate in step (1), and the amount is reduced to 203.5 grams, polyethylene glycol (average molecular weight 1000) Substitute polyvinyl alcohol (average molecular weight 500), reduce the amount to 5 grams, and increase the reaction temperature to 80°C.

[0050] The transmission electron microscope image of the finally obtained silica airgel is as follows: Figure 5 As shown, its size ranges from 5-10 microns, and its internal porosity is high. After drying, no damage to the porous structure was found under high vacuum conditions.

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Abstract

The invention discloses a preparation method for a hydrophilic silicon dioxide aerogel microsphere. Specifically, the preparation method comprises the following steps: 1) adding tetralkoxysilane and hydroxyl-contained hydrophilic compound into a solvent to be evenly dispersed, and adding acid to obtain prepolymer; 2) dispersing in an aqueous phase to carry out self-assembling; 3) adding alkali for washing; 4) drying. The preparation method has the advantages of environment protection, simpleness in operation and low cost. The hydrophilic silicon dioxide aerogel microsphere obtained with the method is provided with a silicon dioxide shell with smaller holes and a silicon dioxide skeleton with a larger-hole structure, wherein the silicon dioxide skeleton is covered in the silicon dioxide shell. The invention also discloses the hydrophilic silicon dioxide aerogel microsphere which has relatively good dispersion performance, and has high adhesive force with a matrix when being applied to a coating.

Description

technical field [0001] The invention relates to the technical field of material technology, in particular to a hydrophilic silica airgel microsphere and a preparation method thereof. Background technique [0002] Airgel is the material with the lowest thermal conductivity known so far, and has high application potential in the field of thermal insulation materials. Airgel belongs to ultra-low density (0.003-0.6g / cm 3 ), ultra-high specific surface area (400-1500m 2 / g), ultra-high porosity (80-99.8%) and ultra-low thermal conductivity (0.013-0.038W / mK) materials, usually extracted from the nanopores of gel materials by supercritical, subcritical and atmospheric drying methods Made out of solvent. The pore size of airgel is generally below 50 nanometers, which is smaller than the mean free path (70 nanometers) of air molecules at normal temperature and pressure. The collision probability between air molecules is very low, and it is difficult to achieve heat conduction, so ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/158
CPCC01B33/1585C01P2002/82C01P2004/03C01P2004/04C01P2004/32C01P2004/61C01P2006/10C01P2006/12
Inventor 赵永亮朱晓敏邱雄豪
Owner 上海特栎材料科技有限公司
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