CN102992333A - Low-cost method for preparing aerosil - Google Patents
Low-cost method for preparing aerosil Download PDFInfo
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- CN102992333A CN102992333A CN2013100003749A CN201310000374A CN102992333A CN 102992333 A CN102992333 A CN 102992333A CN 2013100003749 A CN2013100003749 A CN 2013100003749A CN 201310000374 A CN201310000374 A CN 201310000374A CN 102992333 A CN102992333 A CN 102992333A
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Abstract
The invention belongs to the technical field of nanometer porous material preparation and particularly relates to a low-cost method for preparing aerosol. Low-cost hydrosol serves as a precursor, deionized water serves as a solvent, an acid catalyst is added, surfactants are added, and aerosil with no need of any surface modification and solvent replacement is prepared through a sol-gel process. The aerosil has good heat preservation and heat insulation performances and mechanical performances, the thermal conductivity can be reduced to a lower level, the elasticity modulus can achieve more than 6Mpa, and the aerosil has an equivalent mechanical strength with the mechanical strength of traditional fiber composite aerogel. The method is simple in technology, high in operability and applicable to factory large-scale production and application.
Description
Technical field
The invention belongs to aerogel class technical field of material, relate to the low-cost preparation method with the aerosil that adds solvent replacing loaded down with trivial details in the tensio-active agent replacement aerogel preparation process and finishing step.
Background technology
SiO
2The nano-porous materials that aerogel is a kind of novel low density, transparent, structure is controlled has continuous three-dimensional net structure.Its density is at 3-500mg/cm
3Between adjustable, be the minimum a kind of solid material of density in the world, porosity is up to 99.8%, aperture size is between 1-100nm, specific surface area is up to 1000m
2/ g.It has excellent thermal and insulating performance simultaneously, and thermal conductivity is extremely low under the normal temperature and pressure, be at present known to the minimum solid material of thermal conductivity, be with a wide range of applications in heat preservation and insulation field.
The most supercritical dryings that adopt of aerogel prepare, and cost is high, has a big risk.In order to reduce cost and risk, the method for exploring constant pressure and dry is imperative.Although traditional constant pressure and dry method can be prepared the SiO that density is low, thermal and insulating performance is good equally
2Aerogel, but operating process is loaded down with trivial details, spended time is long, and the gel of preparing need to can be dry through the repeatedly solvent replacing of nearly week age and finishing.Wherein replace needed raw materials cost high, need to constantly use a large amount of surface tension solvent less than water (such as ethanol, hexamethyldisiloxane, normal hexane etc.) to realize the abundant replacement of solvent.And it is low that the aerogel of producing has physical strength, frangible, is not easy the shortcoming of moulding.Because process is loaded down with trivial details, replace the factors such as solvent cost height, can't carry out suitability for industrialized production, every cubic metre almost needs 4-5 ten thousand Renminbi, is not easy to large-scale application.
These deficiencies that exist based on traditional constant pressure and dry method now, we need to constantly explore new method and prepare SiO
2Aerogel.Up to the present, there is not yet document and patent report prepare aerogel class material with interpolation tensio-active agent replacement solvent replacing and finishing step method.This method not only can shorten the aerogel production time greatly, and has avoided loaded down with trivial details solvent replacing and finishing process, has saved replacement solvent and the coating materials of a large amount of costlinesses.In addition, the SiO for preparing of this method
2The mechanical property of aerogel makes moderate progress.Suitable with the composite aerogel physical strength that obtains behind the traditional method conjugated fibre.And simple to operate, technique and skill descends, and this will promote aerogel in the large-scale application of heat preservation and insulation field, realizes suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of with low costly, reaction time is short, and is applied widely, the low-cost preparation method of aerosil that can suitability for industrialized production.
In the situation of the present invention take the water-sol as presoma, adopt water to reduce raw materials cost as solvent, utilization interpolation tensio-active agent reduces the cracking that brings owing to the larger surface tension of water solvent in the constant pressure and dry process and subsides.
The low-cost preparation method of the aerosil that the present invention proposes replaces the low-cost preparation method of the aerogel class material of solvent replacing and finishing step to add tensio-active agent, concrete steps are as follows:
(1) make wet gel take the water-sol, water, catalyzer and tensio-active agent as raw material through sol-gel method, wherein the volume ratio of the water-sol, water, catalyzer is 1:(3 ~ 15): (0.4 ~ 7.4); The mass range of the tensio-active agent that every 10ml water-sol is corresponding is: 0.1 ~ 1g.
(2) wet gel that step (1) is obtained wears out after the drying, namely obtains needed aerosil.
Wherein, the catalyzer described in the step (1) is the catalyzer that can make aqueous sol-gel take hydrofluoric acid as the master.
Tensio-active agent in the step (1) in dodecane base class, tetradecane base class or the n-Hexadecane base class tensio-active agents such as the metal carboxylate take Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, dodecylphosphoric acid sodium as representative, Sulfonates, Sulfates, phosphoric acid salt any.
Constant pressure and dry method in the step (2) be that normal temperature and pressure seasoning, normal pressure Fractional Heat-treatment are dry, heat de-airing is dry or the mode such as lyophilize in any.
The low-cost preparation method of the aerosil that the present invention proposes, to prepare the low-cost preparation method of aerogel class material with suds-stabilizing agent, tensio-active agent, concrete steps are as follows:
(1) take the water-sol, deionized water, catalyzer, tensio-active agent and suds-stabilizing agent as raw material through heated and stirred, leave standstill 1-500min and make wet gel, wherein the volume ratio of the water-sol, deionized water, catalyzer, suds-stabilizing agent is 1:(3 ~ 15): (0.4 ~ 7.4): (0.2 ~ 3), the mass range of the tensio-active agent that every 10ml water-sol is corresponding is: 0.1 ~ 1g.
(2) wet gel that step (1) is obtained wears out after the drying, namely obtains needed aerosil.
Wherein: the Heating temperature described in the step (1) is 30 ℃ ~ 50 ℃.
Tensio-active agent in the step (1) in dodecane base class, tetradecane base class or the n-Hexadecane base class tensio-active agents such as the metal carboxylate take Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, dodecylphosphoric acid sodium as representative, Sulfonates, Sulfates, phosphoric acid salt any.
Constant pressure and dry method in the step (2) be that normal temperature and pressure seasoning, normal pressure Fractional Heat-treatment are dry, heat de-airing is dry or the mode such as lyophilize in any.
Catalyzer described in the step (1) is the catalyzer that can make aqueous sol-gel take hydrofluoric acid as the master.
The SiO of the present invention's preparation
2Aerogel has the characteristics of micron and nano-scale structures concurrently, and is higher in constitutionally stable while activity, successfully solved SiO
2The low cost of aerogel class material prepares a difficult problem.In addition, the adding of tensio-active agent also is conducive to the further raising of its performance.Its raw material is easy to get, and is with low cost, and for fields such as chemical industry and environmental improvements important meaning arranged.
Description of drawings
Fig. 1 is embodiment 2 SiO
2The SEM photo of aerogel.
Fig. 2 is embodiment 2 SiO
2The DMA curve of aerogel.
Fig. 3 is embodiment 2 SiO
2The Fourier transform infrared spectroscopy figure of aerogel.
Embodiment
Reach by the following examples accompanying drawing and further specify the present invention.(each raw material is marketable material, and without specifying, purity is chemical pure or analytical pure grade)
Embodiment 1: aerogel class material preparation
The ratio of the water-sol, deionized water, catalyzer HF and Sodium dodecylbenzene sulfonate is 10ml:30ml:2.32ml:0.228g, adds successively each reactant in well-beaten situation, obtains gel after leaving standstill for some time.Gel placed first 35 ℃ of thermostat containers dry 2 ~ 3 days, placed afterwards 50 ℃ of thermostat containers dry 2 ~ 3 days, descended dry 2 hours at 200 ℃ at last, finally obtained block SiO
2Aerogel material.
Embodiment 2: prepare aerogel class material take sodium lauryl sulphate as tensio-active agent
The ratio of the water-sol, deionized water, catalyzer HF and sodium lauryl sulphate is 10ml:50ml:7.4ml:0.6484g, under 40 ℃ of abundant stirring states, add successively each reactant, until colloidal sol will leave standstill during gel, behind the gel dry 4 ~ 6 days at normal temperatures, in 35 ℃ of thermostat containers dry 1 ~ 2 day afterwards, then in 50 ℃ of thermostat containers dry 2 ~ 3 days, finally can obtain block SiO
2Aerogel material.SEM as shown in Figure 1.Aerogel material Young's modulus at normal temperatures is (as shown in Figure 2) about 9.1MPa, has good mechanical property.Contain in the sample-OH ,-CH
3, the Si-O-SiO such as Si
2The typical group of aerogel (as shown in Figure 3).
Embodiment 3: prepare aerogel class material take Sodium dodecylbenzene sulfonate as tensio-active agent
The ratio of the water-sol, deionized water, catalyzer HF and Sodium dodecylbenzene sulfonate is 10ml:30ml:2.32ml:0.2306g, adds successively each reactant in 35 ℃ of well-beaten situations of heating, obtains gel after leaving standstill.Gel directly places the seasoning of air normal temperature and pressure until quality without obvious reduction, can obtain block SiO
2Aerogel material.
Embodiment 4: aerogel class material preparation
The ratio of the water-sol, deionized water, catalyzer HF and sodium lauryl sulphate is 10ml:50ml:7.4ml:0.6484g, fully adding successively each reactant under the stirring state, obtains gel after leaving standstill.Gel directly places the seasoning of air normal temperature and pressure until quality without obvious reduction, can obtain block SiO
2Aerogel material.
Embodiment 5: prepare aerogel class material take lauryl alcohol as suds-stabilizing agent
The ratio of the water-sol, deionized water, catalyzer HF, suds-stabilizing agent and Sodium dodecylbenzene sulfonate is 10ml:30ml:3ml:0.98:0.23g, adds successively each reactant in 38 ℃ of well-beaten situations of heating, obtains wet gel after leaving standstill.Gel carries out the heat de-airing drying, can obtain block SiO
2Aerogel material.
Embodiment 6: add suds-stabilizing agent and prepare aerogel class material
The ratio of the water-sol, deionized water, catalyzer HF, suds-stabilizing agent and sodium lauryl sulphate is 10ml:50ml:4ml:2ml:0.646g, forms wet gel after heating is added successively each reactant in 38 ℃ of well-beaten situations, left standstill for some time.Gel places 35 ℃ of thermostat container dryings until quality without obvious reduction, can obtain block SiO
2Aerogel material.
Above-described embodiment is only in order to illustrate 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 accordingly; 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 protection scope of the present invention.
Claims (7)
1. the low-cost preparation method of an aerosil is characterized in that concrete steps are as follows:
(1) make wet gel take the water-sol, water, catalyzer and tensio-active agent as raw material through sol-gel method, wherein the volume ratio of the water-sol, water, catalyzer is 1:(3 ~ 15): (0.4 ~ 7.4); The mass range of the tensio-active agent that every 10ml water-sol is corresponding is: 0.1 ~ 1g;
(2) wet gel that step (1) is obtained wears out after the drying, namely obtains needed aerosil.
2. the low-cost preparation method of an aerosil is characterized in that concrete steps are as follows:
(1) take the water-sol, deionized water, catalyzer, tensio-active agent and suds-stabilizing agent as raw material through heated and stirred, leave standstill 1-500min and make wet gel, wherein the volume ratio of the water-sol, deionized water, catalyzer, suds-stabilizing agent is 1:(3 ~ 15): (0.4 ~ 7.4): (0.2 ~ 3), the mass range of the tensio-active agent that every 10ml water-sol is corresponding is: 0.1 ~ 1g;
(2) wet gel that step (1) is obtained wears out after the drying, namely obtains needed aerosil.
3. preparation method according to claim 1 and 2 is characterized in that the catalyzer described in the step (1) is the catalyzer that can make aqueous sol-gel take hydrofluoric acid as the master.
4. preparation method according to claim 2 is characterized in that suds-stabilizing agent described in the step (1) is lauryl alcohol, dodecyl dimethyl ammonium chloride or lauroyl diethanolamine etc. can play steady bubble effect to used tensio-active agent reagent.
5. preparation method according to claim 2 is characterized in that the Heating temperature described in the step (1) is 30 ℃ ~ 50 ℃.
6. preparation method according to claim 1 and 2 is characterized in that the tensio-active agent described in the step (1) is dodecane base class, tetradecane base class or the n-Hexadecane base class tensio-active agents such as the metal carboxylate, Sulfonates, Sulfates, phosphoric acid salt take Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, dodecylphosphoric acid sodium as representative.
7. preparation method according to claim 1 and 2, it is characterized in that the drying means described in the step (2) is the normal temperature and pressure seasoning, the normal pressure Fractional Heat-treatment is dry, heat de-airing is dry or lyophilize in any.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204666A (en) * | 2013-04-22 | 2013-07-17 | 同济大学 | Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost |
| CN103496707A (en) * | 2013-10-09 | 2014-01-08 | 同济大学 | Low-cost preparation method of silica aerogel under pure water system |
| CN104556063A (en) * | 2014-12-30 | 2015-04-29 | 纳诺科技有限公司 | Low-cost preparation method for hydrophobic silica aerogel |
| CN104759285A (en) * | 2015-03-13 | 2015-07-08 | 兰州交通大学 | Preparation method of TiO2/SiO2/Fe3O4 photo-catalyst magnetic fluid |
| CN105693240A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Preparation method of germanium oxide-niobium oxide hybrid aerogel composite material |
| CN108598417A (en) * | 2018-04-24 | 2018-09-28 | 航天特种材料及工艺技术研究所 | A kind of conductive black modification aerosil sulfur loaded composite positive pole and preparation method thereof |
| CN114261986A (en) * | 2022-01-18 | 2022-04-01 | 中国科学技术大学先进技术研究院 | Preparation method of aerogel material and application of aerogel material |
| CN115849862A (en) * | 2022-08-19 | 2023-03-28 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silica aerogel composite material |
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| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
| CN102674375A (en) * | 2012-05-15 | 2012-09-19 | 同济大学 | Method for preparing silica aerogel with low cost in water system |
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| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
| CN102674375A (en) * | 2012-05-15 | 2012-09-19 | 同济大学 | Method for preparing silica aerogel with low cost in water system |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204666A (en) * | 2013-04-22 | 2013-07-17 | 同济大学 | Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost |
| CN103496707A (en) * | 2013-10-09 | 2014-01-08 | 同济大学 | Low-cost preparation method of silica aerogel under pure water system |
| CN104556063A (en) * | 2014-12-30 | 2015-04-29 | 纳诺科技有限公司 | Low-cost preparation method for hydrophobic silica aerogel |
| CN104759285A (en) * | 2015-03-13 | 2015-07-08 | 兰州交通大学 | Preparation method of TiO2/SiO2/Fe3O4 photo-catalyst magnetic fluid |
| CN104759285B (en) * | 2015-03-13 | 2020-06-05 | 兰州交通大学 | TiO 22@SiO2@Fe3O4Preparation method of photocatalytic magnetofluid |
| CN105693240A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Preparation method of germanium oxide-niobium oxide hybrid aerogel composite material |
| CN108598417A (en) * | 2018-04-24 | 2018-09-28 | 航天特种材料及工艺技术研究所 | A kind of conductive black modification aerosil sulfur loaded composite positive pole and preparation method thereof |
| CN108598417B (en) * | 2018-04-24 | 2020-11-13 | 航天特种材料及工艺技术研究所 | Conductive carbon black modified silica aerogel sulfur-loaded composite cathode material and preparation method thereof |
| CN114261986A (en) * | 2022-01-18 | 2022-04-01 | 中国科学技术大学先进技术研究院 | Preparation method of aerogel material and application of aerogel material |
| CN114261986B (en) * | 2022-01-18 | 2023-10-13 | 中国科学技术大学先进技术研究院 | Preparation method of aerogel material and application of aerogel material |
| CN115849862A (en) * | 2022-08-19 | 2023-03-28 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silica aerogel composite material |
| CN115849862B (en) * | 2022-08-19 | 2024-01-30 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silicon aerogel composite material |
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| CN102992333B (en) | 2014-09-17 |
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Effective date of registration: 20170420 Address after: 061108 Cangzhou port chemical industry park in Hebei province by the east of the road to four, south of chemical Avenue Patentee after: Epee and new materials Co., Ltd. Address before: 200092 Shanghai City, Yangpu District Siping Road No. 1239 Patentee before: Tongji University |
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Denomination of invention: Low-cost method for preparing aerosil Effective date of registration: 20200521 Granted publication date: 20140917 Pledgee: Beijing technology intellectual property financing Company limited by guarantee Pledgor: IBIH NEW MATERIAL Co.,Ltd. Registration number: Y2020990000506 |
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Date of cancellation: 20210803 Granted publication date: 20140917 Pledgee: Beijing technology intellectual property financing Company limited by guarantee Pledgor: IBIH NEW MATERIAL Co.,Ltd. Registration number: Y2020990000506 |