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Method for producing silicon dioxide silica aerogel by drying in atmosphere pressure with rice hull as raw material

A technology of atmospheric drying and silica, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of low-grade industrial products and building materials, performance degradation, incomplete carbonization, etc., and achieve pore size distribution The effect of ideal state, reduced equipment requirements, and improved safety performance

Inactive Publication Date: 2008-08-20
纳诺科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

while SiO 2 The surface hydrophobization treatment process of airgel is also the process in which -OH is replaced by hydrophobic groups, and the organosilicon compound orthosilicate [Si(OR) 4 ] or alkyl silicates [R 4-n Si(OR) n ], will make Si(OH) 4 Hydrophobic groups replace the hydroxyl-OH sol in the gel before cross-linking and polymerization, so it is difficult to form a complete gel network structure, resulting in high apparent density and small specific surface area of ​​the airgel prepared by this method.
In addition, organosilicon compound orthosilicate [Si(OR) 4 ] or alkyl silicates [R 4-n Si(OR) n ] reacts violently with water, so adding in the sol stage will inevitably lead to waste of organosilicon compounds, SiO 2 The production cost of airgel increases, and the hydroxyl-OH is difficult to be completely replaced by hydrophobic groups. The product inevitably has hydrophilic problems. It is easy to absorb water during storage and transportation, resulting in performance degradation or even structural collapse. The product is scrapped
[0009] In addition, the incineration and carbonization of rice husk is a difficult process to control
Too low temperature may lead to incomplete carbonization and affect the purity of the product; slightly higher temperature or longer time may cause a large amount of ash, carbonaceous residue or metal residue to remain on the SiO 2 In the pores of the network porous structure, the extracted SiO 2 The highest content can only reach about 98%, and it can only be used for some industrial products and building materials that do not require high purity; increasing the temperature can oxidize impurities, but it cannot guarantee SiO 2 The form does not change from an amorphous state to a crystalline state and loses adsorption performance and destroys the porous network structure
In addition, the incineration process itself is a waste of heat energy, and it is difficult to avoid the release of environmentally harmful gases or smoke during the incineration process, causing environmental pollution and endangering human health.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Mix 100 grams of rice husk with 5.0L of 0.1mol / L NaOH aqueous solution and react at 150°C for 60min under high pressure, and neutralize the filtrate obtained after filtration to pH 10.0 with 2mol / L sulfuric acid; let stand at room temperature for 5 A hydrogel was obtained in minutes. The obtained hydrogel was aged at room temperature for 30 hours, and the ionic water in the hydrogel was replaced with distilled water and ethanol successively. The volume ratio of the solvent to the gel was gel:distilled water:ethanol=1:50:5, time They are 360 ​​hours and 20 hours respectively. Then soak the gel with dimethoxybis(2-methylpropyl)silane at a temperature of 40°C, the volume ratio of dimethoxybis(2-methylpropyl)silane to the gel is 2:1, The time is 10 hours. After taking it out, place it in an oven at 40°C and dry it for 20 hours to obtain a white translucent silica airgel. After testing, its apparent density is 0.082g / cm 3 , the specific surface area is 442m 2 / g, light ...

Embodiment 2

[0048] Mix 100 grams of rice husk with 100ml of 1mol / L NaOH alcohol solution, and heat to 60°C under normal pressure for 120min. Leave for 48 hours to obtain a hydrogel. The obtained hydrogel was aged at 15° C. for 48 hours, and the ionic water in the hydrogel was replaced with ethanol three times, once every 24 hours, and the volume ratio of ethanol to hydrogel was 10:1. Then use dimethoxybis(2-methylpropyl)silane to modify the surface of the hydrogel at 30°C, and the volume ratio of hydrogel to dimethoxybis(2-methylpropyl)silane is 1:3, the time is 48 hours. After drying it in an oven at 25°C for 240 hours, a white translucent silica airgel is obtained. After testing, its apparent density is 0.074g / cm 3 , the specific surface area is 481m 2 / g, light transmittance 79.5%. For hydrophobicity measurement, the product was placed directly on the water surface and weighed after 20 days with a weight gain of 6.7%.

Embodiment 3

[0050] Mix 200 grams of rice husk with 2 L of 0.9 mol / L KOH aqueous solution and boil at normal pressure for 90 minutes. The filtrate obtained after filtration is neutralized to pH 6.5 with an acidic cation exchange resin, filtered again, and allowed to stand at 50°C for 30 minutes. A hydrogel is obtained in minutes. The resulting hydrogel was aged at 50°C for 12 hours, soaked in distilled water for 5 hours in a constant temperature water bath at 80°C, the volume ratio of the amount of distilled water to the gel was 50:1, then soaked the gel with n-heptane, The volume ratio of n-heptane to gel is 10:1, and the time is 1 hour. Soak the gel with a mixture of bistrimethylsiloxymethylsilane and n-heptane, the volume ratio of bistrimethylsiloxymethylsilane, n-heptane, and gel is 1:3:1, The time is 30 minutes. Put it in an oven at 180°C and dry it for 2 hours to obtain a white translucent silica airgel. After testing, its apparent density is 0.054g / cm 3 , with a specific surface...

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PUM

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Abstract

The invention discloses a drying preparation method of silicon dioxide aerogel under atmospheric pressure, using rice husk as raw material, which comprises the following procedures: (1) preparation of rice husk sol; (2) aging of gel; (3) solvent exchange; (4) surface modification of gel; (5) drying under atmospheric pressure. Instead of expensive toxicant organ silicon source, agricultural trashes rice husk is used as raw material, thus greatly reduce the cost; instead of super-critical drying, drying under atmospheric pressure greatly reduces the requirements for the whole process on the equipment, greatly improves the safety performance on one hand, also greatly reduces the running cost on the other. The method in the invention has the advantages of simple technology, easy operation, which is suitable for scale production.

Description

technical field [0001] The invention relates to the field of preparation of chemical materials, in particular to a preparation method of silica airgel. Background technique [0002] Rice husk is a large amount of agricultural waste. my country produces about 200 million tons of rice every year, of which the quality of rice husk accounts for about 20%. Because the rice husk fibrous tissue is covered with hard silicic acid, its nutritional value is extremely low, and its digestible nutrients are all negative, and it is easy to cause gastrointestinal diseases in animals. Due to the high lignin and silicon content, the rice husk is not easy to absorb water, and it is not easy to rot when it is directly applied to the field as fertilizer. This characteristic limits its development and utilization. Now, only a very small amount of rice husk has been utilized. For example, Wenzhou Wusulijiang Rice Industry Co., Ltd. built a power plant with an annual generating capacity of 5 mill...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/157C01B33/146
Inventor 金承黎张洪彪张蓉艳余盛锦
Owner 纳诺科技有限公司
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