CN1557778A - Process for preparation of nano multiporous silicon dioxide aerogel block - Google Patents
Process for preparation of nano multiporous silicon dioxide aerogel block Download PDFInfo
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- CN1557778A CN1557778A CNA2004100160492A CN200410016049A CN1557778A CN 1557778 A CN1557778 A CN 1557778A CN A2004100160492 A CNA2004100160492 A CN A2004100160492A CN 200410016049 A CN200410016049 A CN 200410016049A CN 1557778 A CN1557778 A CN 1557778A
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Abstract
The process of producing silica aerogel block adopts the materials including polysiloxane E-40 as Si source, ethanol, water and hydrofluoric acid; and includes preparing silica aerogel grain via sol-gel and surface modification process at normal pressure, mixing the grain with calcium silicate slurry, rutile type titanium dioxide powder, ceramic fiber, glass fiber and porous cement via powerful stirring, and pressing into block with aerogel content greater than 90 vol%. High strength skeleton may be embedded into the block if necessary. The present invention may be used in insulation, sound isolation and adsorption.
Description
Technical field
The invention belongs to building material technical field, be specifically related to a kind of preparation method of nano porous silicon dioxide aerogel block.
Background technology
SiO
2Aerogel is the low-density porous material of a kind of high-specific surface area, because the existence of nanometer network structure, make this material itself have special nature, have a wide range of applications in various fields such as optics, electricity, acoustics, environmental protection, metallurgy, classified as the world's ten big hot topic science and technology by U.S.'s the 250th phase " science ".Inorganic SiO
2Aerogel has very low solid thermal conduction and can stop the heat conducting nano aperture structure of convection of air, mixes the reflection-absorption ir radiation but utilize, thereby makes SiO
2Aerogel material becomes a kind of efficient and light weight heat-insulation material with utmost point lower thermal conductivity; Also be a kind of outstanding sound insulation, absorption, catalyst support material simultaneously, have wide application prospects.
SiO
2It is raw material that aerogel block body adopts organosilicon usually, prepares in conjunction with the supercritical drying drying method by Sol-Gel technology.
In the application of insulation, sound insulation, sorbing material, can performance, structure, price and the technology that whether possesses suitable volume production be realize large-scale industrial production SiO
2Aerogel and to the important factor of marketing.Because supercritical drying needs the High Temperature High Pressure process, energy consumption is big, and technology is loaded down with trivial details, has certain risk, and product amounts is limited, is unfavorable for suitability for industrialized production, thereby cost is also high.
Traditional SiO
2Aerogel has hindered the development of aerogel in use in market owing to the restriction in appearance forrns and mechanical properties.In fields such as the civil area of routine such as insulation, sound insulation, absorption, all functional the and mechanical property to material itself has proposed certain requirement.When for example using as heat-insulation material, usually need good heat-insulating property, intact structure and cheap price, and traditional asbestos material contains carcinogenic substance, even calcium silicate material can't reach lower heat-insulating property, organic foam class material non-refractory and corrosion, the aerogel cost of overcritical preparation higher and since technology limit can't volume production.
Summary of the invention
The object of the present invention is to provide a kind of technology method for preparing the aerosil block simple, with low cost.
The method for preparing the aerosil block that the present invention proposes is the source with multi-polysiloxane E-40, by technologies such as finishing, constant pressure and dry, briquettings, obtains required aerosil block materials.The preparation concrete steps are as follows;
1, with multi-polysiloxane E-40 and water, ethanol, hydrofluoric acid hybrid reaction, obtains wet gel after 1 ~ 3 hour.The room temperature volume ratio of E-40, ethanol, water, hydrofluoric acid is 1: (3 ~ 15): (0.2 ~ 0.6): (0.03 ~ 0.06).
2, wet gel is immersed in the finishing liquid, normal temperature soaked 20-40 hour down.Finishing liquid is trimethylchlorosilane, normal hexane, Virahol mixed solution, and its room temperature volume ratio is: trimethylchlorosilane: normal hexane: Virahol 1: (8-12): (0.2-0.5).
3, take out wet gel, oven dry is pulverized, and obtaining particle diameter is the hydrophobic type aerosil particle of 2 ~ 5mm.
4, (Φ 2 ~ 5mm) mixes with Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement, and compacting obtains the aerogel composite block, and oven dry gets final product again with gained hydrophobic silica aerogel particle.Each component quality proportioning is: aerogel particle: Calucium Silicate powder slurry: Rutile type Titanium Dioxide: ceramic fiber: glass fibre: honeycombed cement is (10 ~ 200): (10 ~ 50): (4 ~ 6): (0.8 ~ 1.2): (0.4 ~ 0.6).
Change the silica aerogel block by two of the inventive method preparation, its aerogel content is 50-98%.Press the content difference of aerogel, its density is at 109-300kg/m
2Between controlled.Thermal conductivity is 0.025-0.045w/mk in the time of 25 ℃, and high-temperature resistant reaches 1000 ℃.
Among the preparation method of the present invention, can in block, be embedded into high-intensity skeleton, as metallic framework, so that directly use as structured material.
Advantage of the present invention is:
1, adopt melten gel-gel method, finishing technology, under condition of normal pressure the dry aerosil particle that obtains, and form the aerosil block by mixing pressing process.The cost of preparation aerosil block will be starkly lower than traditional supercritical process.
2, possess the nanoporous spacial framework, have performances such as excellent thermal insulation, sound insulation, absorption.
3, shape of product is a complete block, neglects milling train greatly and decides.
4, block possesses whole hydrophobic performance or whole hydrophilicity when use temperature is lower than 250 ℃, and both are adjustable.
5, can be embedded into the high strength skeleton in block central authorities, can directly use as structured material.
Embodiment
The invention is further illustrated by the following examples.
Embodiment 1
Is 1: 8: 0.5 with multi-polysiloxane E-40 and water, ethanol, hydrofluoric acid by the room temperature volume ratio: 0.05 hybrid reaction obtained wet gel after 3 hours.Wet gel is immersed in the finishing liquid (trimethylchlorosilane, normal hexane, Virahol mixed solution, the room temperature volume ratio is: 1: 8: 0.3), and normal temperature soaks down.Take out wet gel after 30 hours,, obtain the hydrophobic type aerogel small-particle of median size Φ 2 ~ 5mm through suitably oven dry pulverizing arrangement.Gained aerosil particle and Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement were pressed mass ratio 100: 10: 5: 1: 1: 0.5, mix through brute force, obtain block after the compacting.Through 105 ℃ of oven dry in 20 hours, obtain whole hydrophobic type aerosil block (aerogel volume content＞90%) again.
Embodiment 2
E-40 and water, ethanol, hydrofluoric acid are 1: 3: 0.2 by the room temperature volume ratio: 0.06; In the finishing liquid, trimethylchlorosilane, normal hexane, Virahol mixed solution, the room temperature volume ratio is: 1: 10: 0.3; Aerosil particle and Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement are 10: 10: 5 by mass ratio: 1: 1: 0.5.All the other conditions obtain whole hydrophobic type aerosil block (aerogel volume content is more than 90%) with embodiment 1.
Embodiment 3
E-40 and water, ethanol, hydrofluoric acid are 1: 15: 0.6 by the room temperature volume ratio: 0.6; In the finishing liquid, trimethylchlorosilane, normal hexane, Virahol mixed solution, the room temperature volume ratio is: 1: 12: 0.5; Aerosil particle and Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement are 200: 50: 6 by mass ratio: 1.2: 1.2: 0.6.All the other conditions obtain whole hydrophobic type aerosil block (aerogel volume content is more than 90%) with embodiment 1.
Embodiment 4:(specifically uses)
Is 100: 10: 5 with aerosil particle and Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement by mass ratio: 1: 1: 0.5, mix through brute force, evenly pour into cylindrical with in the shape goods press, repressed moulding, oven dry in 20 hours obtains overlapping the special-shaped composite block of tubbiness aerogel.
Claims (2)
1, a kind of preparation method of nano porous silicon dioxide aerogel block is characterized in that concrete steps are as follows:
(1) with multi-polysiloxane E-40 and water, ethanol, hydrofluoric acid hybrid reaction, obtains wet gel after 1～3 hour.The room temperature volume ratio of E-40, ethanol, water, hydrofluoric acid is 1: (3～15): (0.2～0.6): (0.03～0.06);
(2) wet gel is immersed in the finishing liquid, normal temperature soaked 20-40 hour down, finishing liquid be trimethylchlorosilane normal hexane, Virahol mixed solution, its room temperature volume ratio is: trimethylchlorosilane: normal hexane: Virahol 1: (8-12): (0.2-0.5);
(3) take out wet gel, oven dry is pulverized, and obtaining particle diameter is the hydrophobic type aerosil particle of 2～5mm;
(4) gained hydrophobic silica aerogel particle and Calucium Silicate powder slurry, Rutile type Titanium Dioxide, ceramic fiber, glass fibre, honeycombed cement are mixed, compacting obtains the aerogel composite block, and oven dry gets final product again; Each component quality proportioning is: aerogel particle: Calucium Silicate powder slurry: Rutile type Titanium Dioxide: ceramic fiber: glass fibre: honeycombed cement is (10～200): (10～50): (4～6): (0.8～1.2): (0.4～0.6).
2, preparation method according to claim 1 is characterized in that being embedded in the block high strength skeleton.
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| CN1317187C (en) * | 2005-07-12 | 2007-05-23 | 北京科技大学 | Process for preparing stephanoporate powder doped silica aerogel heat-insulation material |
| CN100384726C (en) * | 2005-05-19 | 2008-04-30 | 同济大学 | Surface activity adjustable nano porous silicon dioxide aerogel and its preparation method |
| CN100398492C (en) * | 2005-08-01 | 2008-07-02 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN100400153C (en) * | 2005-05-12 | 2008-07-09 | 同济大学 | Composite absorption filtering material contg. porous aerogel, and its prepn. method |
| CN100463864C (en) * | 2006-05-22 | 2009-02-25 | 沈阳建筑大学 | Method for preparing silicon dioxide cold-catalyst water purifying agent |
| CN101948277A (en) * | 2010-09-08 | 2011-01-19 | 广西大学 | Method for preparing light porous inorganic gelled material product from gel particles |
| CN101444739B (en) * | 2008-12-22 | 2011-06-08 | 长沙星纳气凝胶有限公司 | Copper-based nano-catalyst for hydrogen production by ethanol steam reforming and preparation method thereof |
| CN101565296B (en) * | 2009-06-08 | 2011-09-14 | 河北理工大学 | Method for preparing hydrophobic SiO<2>-TiO<2>-ZrO<2> xerogel |
| CN101646622B (en) * | 2007-03-27 | 2012-01-04 | Neb株式会社 | Method for preparing hydrophobic aerogel and hydrophobic aerogel prepared therefrom |
| CN102417363A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micron-nano-sized porous composite material and preparation method thereof |
| CN102417365A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micro-nano porous ceramic composite material and preparation method thereof |
| CN101638237B (en) * | 2008-07-28 | 2012-06-13 | 广东道氏技术股份有限公司 | Method for quickly preparing silicondioxlde aerogel |
| CN102531536A (en) * | 2011-12-20 | 2012-07-04 | 冷水江三A化工有限责任公司 | Flame retardant silica aerogel heat insulation composite material and preparation method thereof |
| CN102659120A (en) * | 2012-04-18 | 2012-09-12 | 同济大学 | Preparation method for hydrophobic large-size bulk nanometer porous SiO2 aerogel |
| CN103172076A (en) * | 2013-03-27 | 2013-06-26 | 中国科学院深圳先进技术研究院 | Preparation method for silicon oxide nano-particles |
| CN101722604B (en) * | 2009-11-30 | 2013-08-21 | 浙江省普瑞科技有限公司 | Method for preparing fiber base material and silicon dioxide aerogel composite heat insulating sleeve |
| CN105503037A (en) * | 2015-12-29 | 2016-04-20 | 葛宏盛 | Nano thermal insulation material and preparing method thereof |
| CN105669101A (en) * | 2009-11-25 | 2016-06-15 | 卡博特公司 | Aerogel composites and methods for making and using them |
| CN105688848A (en) * | 2016-03-12 | 2016-06-22 | 常州大学 | Preparation method of carbon-silicon composite adsorbent |
| CN106007548A (en) * | 2016-06-28 | 2016-10-12 | 蚌埠市方阵商品混凝土有限公司 | Heat insulation concrete |
| CN106431168A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Method for preparing bulk-shaped flexible aerogel through normal-pressure drying |
| CN106517983A (en) * | 2016-10-28 | 2017-03-22 | 北京兆信绿能科技有限公司 | Ceramic nano coating material and preparation method thereof |
| CN107074563A (en) * | 2014-09-25 | 2017-08-18 | 日立化成株式会社 | Aeroge complex, supporting member and heat insulating material with aeroge complex |
| CN107265468A (en) * | 2016-04-08 | 2017-10-20 | 南京唯才新能源科技有限公司 | A kind of aerogel material and its surface modifying method |
| CN107513863A (en) * | 2017-08-01 | 2017-12-26 | 上海工程技术大学 | A kind of preparation method of the netted super-hydrophobic textile of nano compound stephanoporate |
| CN107922738A (en) * | 2015-09-01 | 2018-04-17 | 日立化成株式会社 | Sol composition and aeroge |
| CN109336641A (en) * | 2018-12-17 | 2019-02-15 | 方期洲 | A kind of chemical reaction kettle heat insulating material for external and preparation method thereof |
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- 2004-02-03 CN CNB2004100160492A patent/CN100372812C/en not_active Expired - Fee Related
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| CN100400153C (en) * | 2005-05-12 | 2008-07-09 | 同济大学 | Composite absorption filtering material contg. porous aerogel, and its prepn. method |
| CN100384726C (en) * | 2005-05-19 | 2008-04-30 | 同济大学 | Surface activity adjustable nano porous silicon dioxide aerogel and its preparation method |
| CN1317187C (en) * | 2005-07-12 | 2007-05-23 | 北京科技大学 | Process for preparing stephanoporate powder doped silica aerogel heat-insulation material |
| CN100398492C (en) * | 2005-08-01 | 2008-07-02 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
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| CN103172076A (en) * | 2013-03-27 | 2013-06-26 | 中国科学院深圳先进技术研究院 | Preparation method for silicon oxide nano-particles |
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| CN105503037A (en) * | 2015-12-29 | 2016-04-20 | 葛宏盛 | Nano thermal insulation material and preparing method thereof |
| CN105688848A (en) * | 2016-03-12 | 2016-06-22 | 常州大学 | Preparation method of carbon-silicon composite adsorbent |
| CN107265468A (en) * | 2016-04-08 | 2017-10-20 | 南京唯才新能源科技有限公司 | A kind of aerogel material and its surface modifying method |
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| CN106431168A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Method for preparing bulk-shaped flexible aerogel through normal-pressure drying |
| CN106517983A (en) * | 2016-10-28 | 2017-03-22 | 北京兆信绿能科技有限公司 | Ceramic nano coating material and preparation method thereof |
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| CN109336641A (en) * | 2018-12-17 | 2019-02-15 | 方期洲 | A kind of chemical reaction kettle heat insulating material for external and preparation method thereof |
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