CN102674375A - Method for preparing silica aerogel with low cost in water system - Google Patents
Method for preparing silica aerogel with low cost in water system Download PDFInfo
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- CN102674375A CN102674375A CN2012101492343A CN201210149234A CN102674375A CN 102674375 A CN102674375 A CN 102674375A CN 2012101492343 A CN2012101492343 A CN 2012101492343A CN 201210149234 A CN201210149234 A CN 201210149234A CN 102674375 A CN102674375 A CN 102674375A
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- aerosil
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- deionized water
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- colloidal sol
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Abstract
The invention relates to a method for preparing silica aerogel with low cost in a water system. According to the method, with industrial silica hydrosol as precursor, deionized water as solvent and acid as catalyst, the aerogel is prepared by drying in different ways. The simple preparation method greatly reduces the preparation cost of the silica aerogel, raw materials are chip and easy to obtain, reaction process is simple and controllable, the reaction period is short; and the prepared silica aerogel has lower density and higher porosity.
Description
Technical field
The present invention relates to the preparation field of inorganic amorphous solid-state material, be specifically related to a kind of in aqueous systems
Low-costThe method for preparing aerosil.
Background technology
Nanotechnology be develop rapidly late 1980s one in front of the door along the new branch of science of handing over justice property, be research and utilize structure, characteristic and the interactional new and high technology thereof of atom and molecule on microscale.Nanotechnology is acknowledged as the most promising scientific domain of 21 century.Along with development of science and technology, People more and more is paid attention to Green Chemistry.Green Chemistry is claimed environmental friendliness chemistry, environmentally friendly chemistry, cleaning chemistry again.Three standards of the green synthetic of nano material are to select the solvent system of environmentally safe, reductive agent and nontoxic stablizer for use.
Aerosil is a kind of porous material, and porosity can be up to 99.8%, and bore hole size can be in 1 ~ 100nm scope inner control, and specific surface area can be up to 1000m
2/ g, volume density can be at 3 ~ 500kg/m
3Between regulate.Aerosil essentially consist material is silicon-dioxide (in the earth's crust 87% of silica comprises earth's crust total mass), and environmentally safe meets current people to using the requirement of material, is the type material of a kind of hi-tech, environmental protection.Silicon-dioxide thermal conductivity very low (the minimum 0.015W/ (m# K) that reaches under the normal temperature and pressure) is to know at present minimum a kind of of thermal conductivity in the solid-state material, can be used as thermal insulation material.Again because of its special optics, electricity, acoustics and thermal property, aerosil can be widely used in national defence such as heat preserving and insulating material, the heat insulation window of buildings, solar collector, aerospace and field such as civilian future.
The preparation of traditional silicon dioxide gas gel need use expensive positive silicic acid fat (TEOS, TMOS etc.) to be the silicon source usually; Organism such as ethanol, acetonitrile is a solvent; Adopt complicated dangerous high temperature, high pressure, supercritical fluid drying technology, cost is too high, and is dangerous big; Preparation technology is difficult to control, thereby has hindered the scale operation and the commercialization of this aerogel material greatly.In order to solve the problem of gas gel expensive raw materials and supercritical drying complex process, danger, people attempt novel process from material choice and drying process equal angles.Domestic and international many researchists adopt exchange resin to remove the foreign ion in the water glass at present, obtained the aerosil of excellent performance, but the purification of water glass have increased preparation cost and process complexity equally.Many researchists adopt the surface modification method constant pressure and dry simultaneously, yet the introducing of coating materials makes that whole preparation cost fall is not obvious.
Reduce the cost of silicon source, solvent and drying process simultaneously, avoid introducing new flow process and reagent again, can reduce the preparation cost of aerosil significantly.Service water colloidal sol is a kind of cheap reagent, the service water colloidal sol of same silicone content compare with positive silicic acid fat cost less than hundred ten, service water colloidal sol water soluble can water be a solvent simultaneously, compares with organic solvent, solvent cost reduces greatly.Therefore, be the silicon source with service water colloidal sol, water is solvent, avoids under the situation of finishing, and the cost of aerosil can significantly reduce, and such method is not appeared in the newspapers in present document and patent as yet.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, technology is simple, reaction time is short method that in aqueous systems, prepares aerosil.
The method that in system, prepares aerosil that the present invention proposes, concrete steps are following:
(1) be that 30% industrial alkaline silica sol dilutes with deionized water with massfraction;
(2) in the silicon sol of step (1), add an acidic catalyst under the agitation condition, magnetic agitation 5-10min;
(3) leave standstill 12-24h under the colloidal sol room temperature with step (2) gained, treat colloidal sol generation gel;
(4) gel with step (3) gained carries out drying, gets aerosil;
Wherein: the adding proportion of industrial alkaline silica sol, deionized water, an acidic catalyst is: 10-20ml:20-100ml:0.5-2ml.
Among the present invention, an acidic catalyst described in the step (2) is hydrofluoric acid (HF) or rare nitric acid.
Among the present invention, the drying means described in the step (4) is ethanol supercritical drying or constant pressure and dry.
Utilize the density range of the aerosil that the inventive method prepares to be 85-215mg/cm
3
The present invention realizes that successfully aerosil prepares and constant pressure and dry, has reduced its preparation cost significantly in water system.Prepared aerosil hole forming property is good, and porosity is high, and is simple to operate, for heat insulating, sorbent material building material field important meaning arranged all.
Description of drawings
Fig. 1 low-density silicon dioxide aerogel photo.
Fig. 2 intermediate density aerosil SEM figure.
Fig. 3 high-density aerosil N
2The adsorption desorption curve.
The rare nitric acid catalysis of Fig. 4 aerosil XRD spectrum.
Fig. 5 constant pressure and dry aerosil SEM figure.
Embodiment
Below further specify the present invention through embodiment and accompanying drawing.(each raw material is marketable material, does not have the purity of special instruction and is CP or analytical pure grade).
Embodiment 1: the supercritical drying preparation of low-density silicon dioxide aerogel
The adding proportion of industry alkaline silica sol, deionized water, HF is 30wt%, and 10ml:70ml:1ml progressively adds industrial alkaline silica sol and HF in deionized water under the well-beaten situation, and the stirring heating time is 5min.Wait to stir finish after with leaving standstill colloidal sol generation gel under the colloidal sol room temperature 12 hours.With absolute ethyl alcohol gel is carried out solvent replacing with aging, the replacement digestion time is 6 days.Gas gel is carried out the ethanol supercritical drying, can obtain aerosil, its density is 85mg/cm
3, its photo such as Fig. 1.
Embodiment 2: the supercritical drying preparation of intermediate density aerosil
The adding proportion of industry alkaline silica sol, deionized water, HF is 30wt%, and 20ml:100ml:2ml progressively adds industrial alkaline silica sol and HF in deionized water under the well-beaten situation, and the stirring heating time is 10min.Wait to stir finish after with leaving standstill colloidal sol generation gel under the colloidal sol room temperature 24 hours.With absolute ethyl alcohol gel is carried out solvent replacing with aging, the replacement digestion time is 6 days.Gel is carried out the ethanol supercritical drying, can obtain aerosil, its density is 127mg/cm
3, its SEM characterizes like Fig. 2.
Embodiment 3: the supercritical drying preparation of high-density aerosil
The adding proportion of industry alkaline silica sol, deionized water, HF is 30wt%, and 10ml:20ml:0.5ml progressively adds industrial alkaline silica sol and HF in deionized water under the well-beaten situation, and the stirring heating time is 5min.Wait to stir finish after with leaving standstill colloidal sol generation gel under the colloidal sol room temperature 12 hours.With absolute ethyl alcohol gel is carried out solvent replacing with aging, the replacement digestion time is 6 days.Gel is carried out the ethanol supercritical drying, can obtain aerosil, its density is 215mg/cm
3, its N
2Adsorption desorption curve such as Fig. 3.
Embodiment 4: the preparation of rare nitric acid catalysis aerosil
The adding proportion of industry alkaline silica sol, deionized water, rare nitric acid is 30wt%, 20ml:80ml:13wt%, and 5ml progressively adds industrial alkaline silica sol and rare nitric acid in deionized water under the well-beaten situation, and the stirring heating time is 10min.Wait to stir finish after with leaving standstill colloidal sol generation gel under the colloidal sol room temperature 24 hours.With absolute ethyl alcohol gel is carried out solvent replacing with aging, the replacement digestion time is 6 days.Gel is carried out the ethanol supercritical drying, can obtain aerosil, its XRD spectrum is like Fig. 4.
Embodiment 5: the constant pressure and dry preparation of aerosil
The adding proportion of industry alkaline silica sol, deionized water, HF is 30wt%, and 10ml:40ml:1ml progressively adds industrial alkaline silica sol and HF in deionized water under the well-beaten situation, and the stirring heating time is 5min.Wait to stir finish after with leaving standstill colloidal sol generation gel under the colloidal sol room temperature 12 hours.Gel was placed 60 ° of C isoperibols following 7 days, can obtain aerosil, its SEM characterizes like Fig. 5.
Above-described embodiment has been merely explanation technological thought of the present invention and characteristics; Its purpose is to make those of ordinary skill in the art can understand content of the present invention and implements according to this; The scope of this patent also not only is confined to above-mentioned specific embodiment; Be all equal variation or modifications of doing according to disclosed spirit, still be encompassed in the protection domain of this patent.
Claims (4)
- One kind in aqueous systems Low-costThe method for preparing aerosil is characterized in that concrete steps are following:(1) be that 30% industrial alkaline silica sol dilutes with deionized water with massfraction;(2) in the silicon sol of step (1), add an acidic catalyst under the agitation condition, magnetic agitation 5-10min;(3) leave standstill 12-24h under the colloidal sol room temperature with step (2) gained, treat colloidal sol generation gel;(4) gel with step (3) gained carries out drying, gets aerosil;Wherein: the adding proportion of industrial alkaline silica sol, deionized water, an acidic catalyst is: 10-20ml:20-100ml:0.5-2ml.
- 2. preparation method according to claim 1 is characterized in that used an acidic catalyst is hydrofluoric acid or rare nitric acid.
- 3. preparation method according to claim 1 is characterized in that the said drying means of step (4) is ethanol supercritical drying or constant pressure and dry.
- 4. preparation method according to claim 1, the aerosil density range that it is characterized in that gained is 85-215mg/cm 3
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101492343A CN102674375A (en) | 2012-05-15 | 2012-05-15 | Method for preparing silica aerogel with low cost in water system |
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| CN2012101492343A CN102674375A (en) | 2012-05-15 | 2012-05-15 | Method for preparing silica aerogel with low cost in water system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992333A (en) * | 2013-01-04 | 2013-03-27 | 同济大学 | Low-cost method for preparing aerosil |
| CN109294292A (en) * | 2018-09-14 | 2019-02-01 | 湖南凯斯利新材料有限公司 | A kind of smoke-free and tasteless fire-proof and thermal-insulation moisture gel aqueous inorganic ceramic coating and preparation method thereof |
| CN113548817A (en) * | 2021-06-24 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method, product and application of aerogel composite material |
| CN114538454A (en) * | 2022-01-28 | 2022-05-27 | 江苏安珈新材料科技有限公司 | Method for preparing silica aerogel by using alkaline silica sol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5738801A (en) * | 1993-08-31 | 1998-04-14 | Basf Aktiengesellschaft | Hydrophobic silica aerogels |
| CN101844771A (en) * | 2010-06-14 | 2010-09-29 | 大连理工大学 | Method for preparing super-hydrophobic silica aerogel at normal pressure |
| CN102167337A (en) * | 2011-03-21 | 2011-08-31 | 冷水江三A化工有限责任公司 | Silicon dioxide aerogel and preparation method thereof |
-
2012
- 2012-05-15 CN CN2012101492343A patent/CN102674375A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5738801A (en) * | 1993-08-31 | 1998-04-14 | Basf Aktiengesellschaft | Hydrophobic silica aerogels |
| CN101844771A (en) * | 2010-06-14 | 2010-09-29 | 大连理工大学 | Method for preparing super-hydrophobic silica aerogel at normal pressure |
| CN102167337A (en) * | 2011-03-21 | 2011-08-31 | 冷水江三A化工有限责任公司 | Silicon dioxide aerogel and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 史非: "常压干燥制备SiO2气凝胶及其结构、性能研究", 《中国博士学位论文全文数据库 工程科技I辑》, no. 03, 31 March 2008 (2008-03-31), pages 38 - 39 * |
| 沈军等: "以水玻璃为源常压制备高保温二氧化硅气凝胶", 《功能材料》, vol. 40, no. 1, 31 December 2009 (2009-12-31) * |
| 王冬冬等: "常压干燥法制备SiO2气凝胶粉体", 《耐火材料》, vol. 45, no. 2, 30 April 2011 (2011-04-30), pages 96 - 99 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992333A (en) * | 2013-01-04 | 2013-03-27 | 同济大学 | Low-cost method for preparing aerosil |
| CN102992333B (en) * | 2013-01-04 | 2014-09-17 | 同济大学 | Low-cost method for preparing aerosil |
| CN109294292A (en) * | 2018-09-14 | 2019-02-01 | 湖南凯斯利新材料有限公司 | A kind of smoke-free and tasteless fire-proof and thermal-insulation moisture gel aqueous inorganic ceramic coating and preparation method thereof |
| CN113548817A (en) * | 2021-06-24 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method, product and application of aerogel composite material |
| CN114538454A (en) * | 2022-01-28 | 2022-05-27 | 江苏安珈新材料科技有限公司 | Method for preparing silica aerogel by using alkaline silica sol |
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Application publication date: 20120919 |