CN102992333B - Low-cost method for preparing aerosil - Google Patents
Low-cost method for preparing aerosil Download PDFInfo
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- CN102992333B CN102992333B CN201310000374.9A CN201310000374A CN102992333B CN 102992333 B CN102992333 B CN 102992333B CN 201310000374 A CN201310000374 A CN 201310000374A CN 102992333 B CN102992333 B CN 102992333B
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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 by the low-cost preparation method who adds the aerosil of solvent replacing loaded down with trivial details in 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 under normal temperature and pressure, thermal conductivity is extremely low, be at present known to the minimum solid material of thermal conductivity, in heat preservation and insulation field, be with a wide range of applications.
Prepared by the most supercritical dryings that adopt of aerogel, cost is high, has a big risk.In order to reduce costs 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 dried through repeatedly solvent replacing and the finishing of nearly week age.Wherein replace needed raw materials cost high, need to constantly with a large amount of surface tension solvent less than water (as ethanol, hexamethyldisiloxane, normal hexane etc.), realize the abundant replacement of solvent.And it is low that the aerogel of producing has physical strength, frangible, be not easy the shortcoming of moulding.Because process is loaded down with trivial details, replace the factors such as solvent cost height, cannot 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 constant pressure and dry method based on traditional exists now, we need to constantly explore new method and prepare SiO
2aerogel.Up to the present, there is not yet document and patent report and by interpolation tensio-active agent replacement solvent replacing and finishing step, prepare the method for aerogel class material.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 that this method prepares
2the mechanical property of aerogel makes moderate progress.Suitable with the composite aerogel physical strength obtaining after traditional method conjugated fibre.And simple to operate, technique and skill declines, 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, applied widely, the low-cost preparation method of aerosil that can suitability for industrialized production.
The present invention be take in the situation that the water-sol is presoma, adopts water to reduce raw materials cost as solvent, utilizes to add tensio-active agent and reduce the cracking bringing due to the surface tension that in constant pressure and dry process, water solvent is larger and subside.
The low-cost preparation method of the aerosil that the present invention proposes, to add the low-cost preparation method of the aerogel class material of tensio-active agent replacement solvent replacing and finishing step, concrete steps are as follows:
(1) take the water-sol, water, catalyzer and tensio-active agent makes wet gel through sol-gel method as raw material, and 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 step (1) being obtained carries out, after aging being dried, obtaining needed aerosil.
Wherein, the catalyzer described in step (1) is to take hydrofluoric acid can make the catalyzer of aqueous sol-gel as master.
Tensio-active agent in step (1) is for take in dodecane base class, tetradecane base class or the n-Hexadecane base class tensio-active agents such as metal carboxylate that Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, dodecylphosphoric acid sodium be representative, Sulfonates, Sulfates, phosphoric acid salt any.
Constant pressure and dry method in 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 passes through heated and stirred, standing 1-500min makes 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 step (1) being obtained carries out, after aging being dried, obtaining needed aerosil.
Wherein: the Heating temperature described in step (1) is 30 ℃ ~ 50 ℃.
Tensio-active agent in step (1) is for take in dodecane base class, tetradecane base class or the n-Hexadecane base class tensio-active agents such as metal carboxylate that Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, dodecylphosphoric acid sodium be representative, Sulfonates, Sulfates, phosphoric acid salt any.
Constant pressure and dry method in 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 step (1) is to take hydrofluoric acid can make the catalyzer of aqueous sol-gel as master.
SiO prepared by the present invention
2aerogel has the feature of micron and nano-scale structures concurrently, higher in constitutionally stable while activity, has successfully solved SiO
2the low cost of aerogel class material is prepared a difficult problem.In addition, adding of tensio-active agent, is also conducive to the further raising of its performance.Its raw material is easy to get, with low cost, and has important meaning for fields such as chemical industry and environmental improvements.
Accompanying drawing explanation
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
By the following examples and accompanying drawing further illustrate the present invention.(each raw material is marketable material, and without special instruction, purity is chemical pure or analytical pure grade)
Embodiment 1: the preparation of aerogel class material
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, after standing for some time, obtains gel.Gel is first placed in 35 ℃ of thermostat containers dry 2 ~ 3 days, is placed in afterwards 50 ℃ of thermostat containers dry 2 ~ 3 days, finally at 200 ℃, is dried 2 hours, finally obtains block SiO
2aerogel material.
Embodiment 2: the sodium lauryl sulphate of take is prepared aerogel class material 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 is standing will gel time, after gel, be dried 4 ~ 6 days at normal temperatures, in 35 ℃ of thermostat containers, be dried 1 ~ 2 day afterwards, then in 50 ℃ of thermostat containers, be dried 2 ~ 3 days, finally can obtain block SiO
2aerogel material.SEM as shown in Figure 1.Aerogel material Young's modulus is at normal temperatures 9.1MPa left and right (as shown in Figure 2), has good mechanical property.In sample, contain-OH ,-CH
3, the SiO such as Si-O-Si
2the typical group of aerogel (as shown in Figure 3).
Embodiment 3: the Sodium dodecylbenzene sulfonate of take is prepared aerogel class material 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, after heating is added successively each reactant in 35 ℃ of well-beaten situations, be standing, obtains gel.Gel is directly placed in the seasoning of air normal temperature and pressure until quality, without obvious reduction, can obtain block SiO
2aerogel material.
Embodiment 4: the preparation of aerogel class material
The ratio of the water-sol, deionized water, catalyzer HF and sodium lauryl sulphate is 10ml:50ml:7.4ml:0.6484g, fully under stirring state, is adding successively each reactant, obtains gel after standing.Gel is directly placed in the seasoning of air normal temperature and pressure until quality, without obvious reduction, can obtain block SiO
2aerogel material.
Embodiment 5: the lauryl alcohol of take is prepared aerogel class material 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, after heating is added successively each reactant in 38 ℃ of well-beaten situations, be standing, obtains wet gel.It is dry that gel carries out heat de-airing, 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, in 38 ℃ of well-beaten situations of heating, adds successively each reactant, after standing for some time, forms wet gel.It is dry until quality, without obvious reduction, can obtain block SiO that gel is placed in 35 ℃ of thermostat containers
2aerogel material.
Above-described embodiment is only in order to illustrate technological thought of the present invention and feature; its object is to make those of ordinary skill in the art can understand content of the present invention and implement accordingly; the scope of this patent is also not only confined to above-mentioned specific embodiment; be all equal variation or modifications of doing according to disclosed spirit, be still encompassed in protection scope of the present invention.
Claims (3)
1. a low-cost preparation method for 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 passes through heated and stirred, standing 1-500min makes wet gel, described Heating temperature is 30 ℃ ~ 50 ℃, 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 step (1) being obtained carries out, after aging being dried, obtaining needed aerosil;
Suds-stabilizing agent described in step (1) is that lauryl alcohol, dodecyl dimethyl ammonium chloride or lauroyl diethanolamine play the reagent of steady bubble effect to tensio-active agent used; Described tensio-active agent be in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate or dodecylphosphoric acid sodium any.
2. preparation method according to claim 1, is characterized in that the catalyzer described in step (1) is to take hydrofluoric acid as instigating the catalyzer of aqueous sol-gel.
3. preparation method according to claim 1, it is characterized in that the drying means described in step (2) is that normal temperature and pressure seasoning, normal pressure Fractional Heat-treatment are dry, heat de-airing is dry or lyophilize in any.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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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 |