CN103204666A - Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost - Google Patents
Method for preparing aerogel or aerogel-fiber composite material in aqueous condition with low cost Download PDFInfo
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Abstract
The invention relates to a method for preparing an aerogel or aerogel-fiber composite material in an aqueous condition with low cost. The preparation method comprises the following steps of: (1) the preparation by adding a surface active agent into silica sol; (2) the preparation by adding a surface active agent-silica sol complex into an inorganic refractory fiber felt or a fiber prefabricated member in a water system; and (3) carrying out normal-pressure aging and drying treatment. The method for preparing the aerogel material is simple in process, strong in operability and low in preparation cost, and does not need organic solvent replacement, modification by a surface modifier, and drying by supercritical equipment. The aerogel and the aerogel-fiber composite material prepared by the method provided by the invention have good mechanical property and good thermal insulation and heat preservation performances, and has the elastic modulus capable of reaching 8MPa; the preparation of the aerogel-fiber composite material enables the pure aerogel with certain contraction to restore to form a complete block, thereby being more conductive to large-scale application; and the aerogel and the aerogel-fiber composite material prepared by the method provided by the invention are excellent in performance, low in cost, and good in industrial production and application prospects.
Description
Technical field
The present invention relates in a kind of aqueous systems to add the preparation method that tensio-active agent is used for aerogel and matrix material thereof, especially a kind of relating to the inorganic fibre is the low-cost method for preparing aerogel or aerogel fibre composite under the aqueous conditions of substrate.
Background technology
Initial SiO
2Aerogel formed wet gel in 1931 by HCl catalytic hydrolysis water glass by Kistler and also prepares through supercritical fluid drying (SCFD) process.This complex manufacturing technology, purification difficult, thereby limited its application.During to the sixties, Nicolaon etc. are presoma with the silicon alkoxide, and alcohol is solvent, prepare gel with a step sol-gel method, prepare aerogel by the SCFD process again.This process has solved issues of purification, has omitted the solvent replacing step, carries out but pure add-on can hinder polycondensation too much, thereby can not realize collosol and gel to transform and the generation wet gel.Afterwards, occur two step method again and prepared the SiO2 aerogel, and can under atmospheric pressure environment, prepare well behaved SiO2 aerogel.This preparation aerosil has two kinds of aging drying meanss: a kind of is that ethanol covers replacement, passes through supercritical drying again.Another kind remains ethanol and covers replacement, again through modifying the back constant pressure and dry.But owing to this dual mode all needs to consume other reagent such as a large amount of alcohol and modifier, and the aging replacement cycle is all very long.This has just caused the preparation cost height of aerosil, needs to consume lot of manpower and material resources, and faces problems such as inflammable, explosive, is difficult to obtain in daily life practical application.
How obtaining low-density silicon dioxide aerogel and it is widely used in the middle of our daily life is to need the problem that solves and consider now.Be to solve the complicated processes that traditional preparation process is brought, this patent mainly is to be solvent with deionized water, replaces ethanol and other modifiers to the processing of gel with adding tensio-active agent and suds-stabilizing agent, and the process normal pressure drying mode that wears out prepares aerogel again.Can reduce preparation cost in a large number like this, also can shorten the cycle greatly, facility simple to operate is conducive to the use of our daily life more.
It is solvent with the deionized water that colloidal sol is made aerogel.Because moisture can evaporate when constant pressure and dry, then the aerogel of Xing Chenging mainly is by the volume decision of reaction solution beyond the deionizing water.
Tensio-active agent is thereby that a kind of condition of surface that can reduce solvent (being generally water) surface tension (or liquid-liquid interface tension force) greatly change system produces pharmaceutical chemicalss wetting and dewetting, emulsification and breakdown of emulsion, dispersion and gel, foaming and a series of effects such as froth breaking and solubilising.The classification situation different according to tensio-active agent adopts the mode of acid catalysis, base catalysis or soda acid two-step catalysis to obtain required aerogel respectively.Another one tensio-active agent preferably just can reach the absorption state of saturation when its concentration is rarer, minimum table (boundary) surface tension is just arranged when namely concentration is rarer.
Science and technology develops rapidly, and is more and more harsher to the demand of material, particularly some performances under the high temperature.As chemical stability, structural stability etc.Many studies show that, the fiber composite aerogel has extremely strong potential ability in the middle of practical application.Mullite fiber for example, it is the novel inorganic fiber that grows up in the later stage seventies 20th century.Mullite fiber structurally is the form existence with mullite (3Al2O32SiO2) dimension crystalline phase, and mullite is stable phase, active low mutually, ties ability again, and the grain-size grain is little.It not only has the advantage of strong height, high-modulus, and high thermal resistance is good, and creep resistance and heat-shock resistance also improve a lot.Can effectively improve the intensity of aerogel and reduce the contraction of gel when dry and pyroprocessing.Thereby fibre composite is widely used in aerospace, military project and high-tech civil area.Become one of the focus in investigation of materials field, various countries in recent years.
At present, existing patent has been told about the preparation of fiber composite alcohol system colloidal sol, but the preparation of fiber composite aqueous systems sol material is not arranged yet.Interpolation tensio-active agent and suds-stabilizing agent can reduce the surface tension in the collosol and gel, are zero but can not make surface tension.And inorganic fibre has high temperature resistant and the strong feature of elastic force.So the inorganic fibre complex water body is colloidal sol the gel that adds the certain contraction of tensio-active agent generation is restored to the original state, the negative impact of avoiding surface tension to bring, thus form complete block.
Add suds-stabilizing agent speed of reaction is increased, reaching the needed time of gelation point shortens relatively, makes also that simultaneously the aerogel structure of preparation is more even, global density little than with suds-stabilizing agent.
The aerogel that makes by colloidal sol-gelation process and the aging drying treatment of normal pressure is a kind of nano-porous materials of controllable structure, and its adjustable density is a kind of more satisfactory low density foam material.The gained aerogel has the continuous three-dimensional network structure, the concrete structure that becomes to loosen of silicon dioxide granule, and border, hole distribution uniform.In addition, the aging drying treatment aerogel of normal pressure is succinct, easy to operate.Do not have supercritical drying to handle loaded down with trivial details control condition, be convenient to large-scale practical application more.
Summary of the invention
The object of the present invention is to provide the silica aerogel that has good heat-proof quality and mechanical property under a kind of aqueous systems and the low-cost industrialized process for preparing of matrix material thereof.
For achieving the above object, the present invention adopts the constant pressure and dry method by silicon sol and tensio-active agent are mixed in proportion, and forms to have the nanoporous network structure, the silica aerogel of high temperature resistant, low thermal conductivity and excellent mechanical performances.And with the silicon sol under the gained aqueous systems and fiber composite, utilize the elastic skeleton structure of fiber, and improve the intensity of aerogel and reduce the contraction of gel in drying process, it is littler to obtain contraction, the aerogel composite that physical strength is higher.
The low-cost method for preparing aerogel under the aqueous conditions that the present invention proposes, concrete steps are as follows:
(1) silicon dioxide gel adds the preparation of tensio-active agent
Be precursor with the silicon sol, add deionized water, catalyzer, tensio-active agent and suds-stabilizing agent, the volume ratio of silicon sol, deionized water, catalyzer and suds-stabilizing agent is 1:(2 ~ 18): (0.5 ~ 10): the mass range of the tensio-active agent of (0.2 ~ 10) every 10ml silicon sol correspondence is: 0.05 ~ 2.5g, by heating unit mixed solution is warming up to 15-45 degree, constant temperature stirs after 5-180 minutes and leaves standstill, after colloidal sol is cooled to room temperature, obtain silicon dioxide gel;
(2) the aging drying treatment of normal pressure
Silicon sol aging drying treatment under normal pressure with preparing namely gets desired product.
The low-cost method for preparing the aerogel fibre composite under the aqueous conditions that the present invention proposes, concrete steps are as follows:
(1) silicon dioxide gel adds the preparation of tensio-active agent
Be precursor with the silicon sol, add deionized water, catalyzer, tensio-active agent and suds-stabilizing agent, the volume ratio of silicon sol, deionized water, catalyzer, tensio-active agent and suds-stabilizing agent is 1:(2 ~ 18): (0.5 ~ 10): (0.2 ~ 10), the mass range of the tensio-active agent of every 10ml silicon sol correspondence is: 0.05 ~ 2.5g; By heating unit mixed solution is warming up to 15-45 degree, constant temperature stirs after 5-180 minutes and leaves standstill, colloidal sol is cooled to room temperature after, obtain silicon dioxide gel;
(2) preparation of fiber reinforcement silicon gel complex material
In reinforcing fiber mats or fiber preform mould are housed, add the silicon dioxide gel that step (1) obtains, make it and blending in of fibers, at room temperature leave standstill 0.5-48 hours after, form gel, obtain fiber reinforcement silicon gel complex material;
(3) the aging drying treatment of normal pressure
Matrix material aging drying treatment under normal pressure with step (2) prepares namely gets desired product.
Among the present invention, reinforcing fiber mats or fiber preform are by any constitutes in resistant to elevated temperatures pure aluminium silicate, mullite, silica fiber, Zirconium oxide fibre, sapphire whisker, carbon fiber or the silicon carbide fiber described in the step (2), Fibre diameter is 3-10 μ m, fiber volume fraction 3%-10%, staple length 0.5-10cm.
Among the present invention, under the described normal pressure method of aging drying treatment be normal temperature and pressure weather aging drying treatment, normal pressure stage by stage in aging heat treatment drying treatment, the aging drying treatment of heat de-airing, freezing aging drying treatment, the aging drying of infrared radiation or the aging drying treatment of air blast any.
Among the present invention, described silicon sol be in the silicon water-sol or the water glass any.
Among the present invention, described catalyzer be among hydrofluoric acid, hydrochloric acid, nitric acid, sulfuric acid, acetic acid, oxalic acid, ammoniacal liquor or the NaOH any.
Among the present invention, described tensio-active agent is any in anion surfactant, fluorine surfactant, amphoterics or the polymeric surface active agent.
Among the present invention, described suds-stabilizing agent be in lauryl alcohol, hexalin or the lauroyl diethanolamine any.
Among the present invention, the surface tension of described tensio-active agent in deionized water solvent is more little, then more is conducive to reduce the aerogel shrinking percentage, increases its porosity, close to the effect of supercritical drying gained.Tensio-active agent can be any in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, Trombovar, tetradecyl benzene sulfonic acid sodium salt, fluorine surfactant, amphoterics, the polymeric surface active agent.
Among the present invention, described suds-stabilizing agent is for the bubble retention time that produces in the colloidal sol that makes preparation increases relatively, reduces deionized water solvent the contacting of when evaporation and silicon sol with this, and reduction total surface tension force is to the influence of gel.Therefore suds-stabilizing agent can be in lauryl alcohol, hexalin, the lauroyl diethanolamine any.
The interpolation tensio-active agent can reduce the surface tension in the colloidal sol greatly, is zero but can not make its surface tension.So prepared sample more or less all can have certain contraction.Because disappear at solvent evaporates rear surface tension force, gel has certain bounce-back.Therefore the wherein more many more easy bounce-backs of hydrophobic grouping generally need finishing to introduce hydrophobic grouping.And the method for adding tensio-active agent does not enter hydrophobic grouping, has just reduced surface tension.And this moment, fiber just played the effect that is similar to hydrophobic grouping, can make the aerogel of preparation form complete block structure.
Beneficial effect of the present invention is: this method technology for preparing aerogel material is simple, workable, need not that organic solvent is replaced and the modification of coating materials, and need not overcritical equipment drying, and preparation cost is cheap.Aerogel and the fibre composite thereof of present method preparation have good mechanical property, and Young's modulus can reach 8MPa, and has good thermal and insulating performance.Wherein the preparation of fibre composite can make the pure aerogel with certain contraction recover former state, forms complete block, more is conducive to large-scale application.Use aerogel and the fibre composite excellent property thereof of the present invention's preparation, with low cost, have favorable industrial production application prospect.
Description of drawings
Fig. 1 is the BET picture of embodiment 1 aerogel.
Fig. 2 is the SEM picture of embodiment 3 silica aerogels.
Fig. 3 is embodiment 4 mullite fiber composite sample pictorial diagram.
Fig. 4 is the SEM picture of embodiment 5 aluminum silicate fiber composite aerogels.
Fig. 5 is the SEM picture of embodiment 6 ceramic fiber composite aerogels.
Embodiment
The invention will be further described by the following examples, but these embodiment must not be used for explaining limiting the scope of the invention.
Embodiment 1: add sodium lauryl sulphate and prepare aerosil class material
The amount ratio of the water-sol, deionized water, catalyzer HF, sodium lauryl sulphate, lauryl alcohol is 10ml:50ml:7.4ml: 0.65g:0.2ml.Earlier the water-sol and deionized water mixing are heated with stirring to 38 ℃, add each reactant more successively, stir and obtain wet gel after for some time is left standstill in the above sealing of 15min.Gel directly places room temperature environment not have considerable change again until quality.Be final required block SiO2 aerogel material.After block aerogel sample mill become regular solid, with volume calculated after its size of vernier caliper measurement, accurately claim its quality with electronic balance, the density that draws this aerogel is 270mg/cm, specific surface area, pore volume, pore size distribution and adsorption desorption thermoisopleth with N2 adsorption desorption instrument working sample, the mean pore size of measuring gel is 8.15nm, and specific surface area is 113m2/g(Fig. 1).
Embodiment 2: amphoterics is used for the preparation of aerogel class material
The amount ratio of the water-sol, deionized water, catalyst n aOH, amphoterics (mainly based on sodium dodecyl aminopropionitrile), hexalin is 10ml:25ml:0.3ml: 1.3 g:2ml.Under the water-sol and 30 ℃ of well-beaten situations of constant temperature of deionized water mixing solutions, add each reactant successively, stir and to leave standstill for some time behind the 60min and obtain gel.Gel has been placed constant wind speed window place, until gel quality affects considerable change has taken place no longer.The block SiO2 aerogel material of final acquisition.Sample has the typical amorphous state structure of SiO2 aerogel.
Embodiment 3: add lauroyl diethanolamine and prepare aerogel class material
The amount ratio of water glass, deionized water, acetic acid, tetradecyl benzene sulfonic acid sodium salt, lauroyl diethanolamine, ammoniacal liquor is 10ml:30ml:1.5ml: 0.14g:2.5ml:1.5ml, earlier the water-sol and deionized water are stirred under 15 ℃ of constant temperature, add acetic acid, tetradecyl benzene sulfonic acid sodium salt then, add lauroyl diethanolamine and ammoniacal liquor (37%) again more than the stirring 10min.Leave standstill until gel more than continuing to stir 20min.Gel placed earlier under the room temperature environment 1 ~ 2 day, put into 35 ℃ of thermostat containers drier 2 ~ 5 days, put into that 50 ℃ of thermostat containers are dry not to have considerable change until quality again, can obtain block SiO
2Aerogel material.By scanning electron microscope sem photo (Fig. 2) as can be known, the aperture of the aerosil of preparation is bigger, and between 500 nanometers, the network skeleton particle is also bigger, is about tens nanometers in several nanometers.
Embodiment 4: the preparation of mullite fiber composite aerogel class material
The amount ratio of the water-sol, deionized water, catalyst ammonia water, fluorine surfactant, hexalin is 10ml:50ml:2ml:0.05g:0.2ml.Be heated under 26 ℃ of well-beaten situations at the water-sol, deionized water mixing solutions and add each reactant successively, be poured in the mould that is placed with mullite fiber after stirring 15min, leave standstill until its gel.Place 40 ℃ of thermostat containers dryings not have obvious reduction until quality again, can obtain fiber composite SiO
2Aerogel material.The composite aerogel plasticity is good, is complete block (Fig. 3).Sample is 8MPa through the Young's modulus that dynamic properties analyser (DMA) test obtains under the normal temperature.
Embodiment 5: the preparation of aluminum silicate fiber composite aerogel class material
The amount ratio of water glass, deionized water, catalyzer HF, Trombovar, lauryl alcohol is 10ml:15ml:1.5ml:0.325g:0.2ml.Under water glass and the well-beaten situation of deionized water mixing solutions, add each reactant successively, be poured in the mould of taking advantage of aluminum silicate fiber behind the stirring 30min, leave standstill until its gel.Gel placed 35 ℃ of thermostat containers earlier dry 2 ~ 3 days, placed 50 ℃ of thermostat containers afterwards dry 2 ~ 3 days, descended dry 2 hours at 200 ℃ at last, finally obtained fiber composite SiO2 aerogel material.By SEM photo (Fig. 4) as seen, aluminum silicate fiber is compounded in the aerogel uniformly.
Embodiment 6: the preparation of ceramic fiber composite aerogel class material
The mol ratio of water glass, deionized water, Sodium dodecylbenzene sulfonate, lauryl alcohol, hydrochloric acid is 10ml:40ml:0.540g:0.5ml:1.5ml, earlier above reagent is mixed successively, after stirring 5min under 38 ℃, add the mixing solutions of deionized water 5ml and strong aqua (37%) 2.7ml again.After continuing to stir for some time colloidal sol is poured in the mould of taking advantage of ceramic fiber, left standstill then and treat its gel.Gel directly places the seasoning of air normal temperature and pressure not have obvious reduction until quality, can obtain fiber composite SiO
2Aerogel material.By scanning electron microscope sem as can be known, gel and fiber composite even (Fig. 5).
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 (8)
1. the low-cost method for preparing aerogel under the aqueous conditions is characterized in that concrete steps are as follows:
(1) silicon dioxide gel adds the preparation of tensio-active agent
Be precursor with the silicon sol, add deionized water, catalyzer, tensio-active agent and suds-stabilizing agent, the volume ratio of silicon sol, deionized water, catalyzer and suds-stabilizing agent is 1:(2 ~ 18): (0.5 ~ 10): (0.2 ~ 10), the mass range of the tensio-active agent of every 10ml silicon sol correspondence is: 0.05 ~ 2.5g; By heating unit mixed solution is warming up to 15-45 degree, constant temperature stirs after 5-180 minutes and leaves standstill, colloidal sol is cooled to room temperature after, obtain silicon dioxide gel;
(2) the aging drying treatment of normal pressure
Silicon sol aging drying treatment under normal pressure with preparing namely gets desired product.
2. the low-cost method for preparing the aerogel fibre composite under the aqueous conditions is characterized in that concrete steps are as follows:
(1) silicon dioxide gel adds the preparation of tensio-active agent
Be precursor with the silicon sol, add deionized water, catalyzer, tensio-active agent and suds-stabilizing agent, the volume ratio of silicon sol, deionized water, catalyzer and suds-stabilizing agent is 1:(2 ~ 18): (0.5 ~ 10): (0.2 ~ 10), the mass range of the tensio-active agent of every 10ml silicon sol correspondence is: 0.05 ~ 2.5g; By heating unit mixed solution is warming up to 15-45 degree, constant temperature stirs after 5-180 minutes and leaves standstill, colloidal sol is cooled to room temperature after, obtain silicon dioxide gel;
(2) preparation of fiber reinforcement silicon gel complex material
In reinforcing fiber mats or fiber preform mould are housed, add the silicon dioxide gel that step (1) obtains, make it and blending in of fibers, at room temperature leave standstill 0.5-48 hours after, form gel, obtain fiber reinforcement silicon gel complex material;
(3) the aging drying treatment of normal pressure
Matrix material aging drying treatment under normal pressure with step (2) prepares namely gets desired product.
3. method according to claim 1 and 2, the method that it is characterized in that aging drying treatment under the described normal pressure be normal temperature and pressure weather aging drying treatment, normal pressure stage by stage in aging heat treatment drying treatment, the aging drying treatment of heat de-airing, freezing aging drying treatment, the aging drying of infrared radiation or the aging drying treatment of air blast any.
4. according to the low-cost method for preparing the aerogel fibre composite under claim 2 aqueous conditions, it is characterized in that reinforcing fiber mats described in the step (2) or fiber preform are by any constitutes in resistant to elevated temperatures pure aluminium silicate, mullite, silica fiber, Zirconium oxide fibre, sapphire whisker, carbon fiber or the silicon carbide fiber, Fibre diameter is 3-10 μ m, fiber volume fraction 3%-10%, staple length 0.5-10cm.
5. method according to claim 1 and 2, it is characterized in that described silicon sol be in the silicon water-sol or the water glass any.
6. method according to claim 1 and 2, it is characterized in that described catalyzer be among hydrofluoric acid, hydrochloric acid, nitric acid, sulfuric acid, acetic acid, oxalic acid, ammoniacal liquor or the NaOH any.
7. method according to claim 1 and 2 is characterized in that described tensio-active agent is any in anion surfactant, fluorine surfactant, amphoterics or the polymeric surface active agent.
8. method according to claim 1 and 2, it is characterized in that described suds-stabilizing agent be in lauryl alcohol, hexalin or the lauroyl diethanolamine any.
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