CN103011745A - Silicon-dioxide aerogel heat insulation composite material and preparation method thereof - Google Patents
Silicon-dioxide aerogel heat insulation composite material and preparation method thereof Download PDFInfo
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- CN103011745A CN103011745A CN2012104946297A CN201210494629A CN103011745A CN 103011745 A CN103011745 A CN 103011745A CN 2012104946297 A CN2012104946297 A CN 2012104946297A CN 201210494629 A CN201210494629 A CN 201210494629A CN 103011745 A CN103011745 A CN 103011745A
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Abstract
The invention provides a fiber-reinforced silicon-dioxide aerogel heat insulation composite material and a preparation method thereof. According to the preparation method, mineral fibers with high mechanical strength, low heat conductivity and good heat stability serve as a reinforcing phase, silicon alcoholate serves as a precursor, fiber-composite silicon-dioxide wet gel is prepared by adopting an acid-base two-step catalysis method, and the block-shaped fiber-reinforced silicon-dioxide aerogel heat insulation composite material is then obtained through aging, modification, solvent displacement and supercritical drying. The prepared aerogel heat insulation composite material has the advantages of excellent mechanical property, good heat-insulating property and higher heat resistance. The aerogel composite material has a three-dimensional porous network-like structure, the compatibility between fibers and an aerogel matrix is good, the interfacial bonding is firm, and no obvious interfaces exist; and according to the block-shaped aerogel composite material, the density is 0.15-0.25 g/cm<3>, the compressive strength is 10%, the strain energy reaches 0.4-2.0MPa, and the coefficient of heat conductivity is 0.016-0.027 W/mK.
Description
Technical field
The invention belongs to field of material preparation, relate to a kind of silicon dioxide aerogel heat-insulating composite material and preparation method.
Background technology
Aerosil makes it all show unique character at aspects such as calorifics, optics, electricity, acoustics with its unique nano-porous structure.Aspect calorifics, the heat transmission is mainly by three approach, and solid thermal conduction, air heat conduct and radiation thermal conduction, because the aerosil void content generally can reach more than 90%, density is low, has special porous network structure.The one side solid phase accounts for whole aerogel volume ratio crooked route little and network structure and has all stoped to a great extent the solid thermal conduction, aerosil is mesoporous material on the other hand, pore is distributed in 50nm once mostly, mean free path 70nm less than air molecule, so that the interstitial air molecule of aerogel is difficult to bump, so the air heat conduction is also very little, last radiation thermal conduction can be stoped by adding opalizer, and these factors have determined that all aerogel is good lagging material.But, SiO
2The characteristics such as the network structure of aerogel uniqueness, high porosity and low density have also caused itself poor mechanical property, so in a lot of fields, SiO
2Aerogel is difficult is used widely as lagging material, need to strengthen just it to reach desirable result of use.
The preparation aspect of aerogel composite heat-insulated material generally has two kinds, a kind of is the gel molding in integral, this method is to introduce wild phase in sol-gel process, directly obtain at last the Monolithic aerogel composite heat-insulated material, publication number provides glass fibre to strengthen the preparation method of silicon dioxide silica aerogel composite material for the Chinese patent application of CN101973752A, selecting diameter is that the glass fibre of 3～8 μ m is as wild phase, fiber after the surface treatment is directly mixed with silicon sol, through ammonia-catalyzed, aging, surface modification, drying obtains block glass fibre and strengthens silicon dioxide silica aerogel composite material, the inorganic fibres such as glass fibre not only price are high, and fiber is generally thicker, Fibre diameter can reach micron order, causes heat-proof quality bad; Publication number provides brucite fiber to strengthen the preparation method of silicon dioxide silica aerogel composite material for the Chinese patent application of CN1803602A, take natural brucite as wild phase has prepared block silicon dioxide silica aerogel composite material, but the natural brucite use temperature is low, and reliable use temperature only has 400 ℃.Another kind is the grain forming method, prepares first nano-hole aerogel particle powder, and then adds wild phase and additive, makes at last the complex body of post forming by mold pressing or casting.Adopting the grain forming method is to make more even that particle mixes with wild phase, generally will introduce additive, such as tackiness agent.Publication number provides a kind of composite manufacture method that contains fiber for CN1196036A China patent application, the method select particle diameter greater than the aerogel particle of 0.5mm as matrix, add fiber and binding agent, under certain temperature and pressure, make the fiber aerogel composite, yet add the solid thermal conduction that tackiness agent can increase material, and aerogel particle and wild phase combine by mold pressing or casting, so that structure is not very even, therefore there are more micropore and macropore in the material structure, the air heat conduction of material is increased, and structure inhomogeneous also may cause producing internal stress in material structure, and the mechanical property of material also can be influenced.
Therefore preparing high performance aerogel composite heat-insulated material is the problem of at present needs solution.
Summary of the invention
The object of the present invention is to provide a kind of fiber-reinforcement silicon dioxide aerogel heat-insulation composite material and preparation method thereof, the employing physical strength is high, thermal conductivity is low, the good mineral fibre of thermal stability is as wild phase, and the aerogel heat-proof composite material that makes has excellent mechanical property, good heat-insulating property and higher thermotolerance.
Technical scheme of the present invention is as follows:
A kind of preparation method of fiber-reinforcement silicon dioxide aerogel heat-insulation composite material, step is as follows:
1) pre-treatment of fiber: mineral fibre places the acid solution stir process, then fiber filter, washing, drying is obtained acid treated fiber; Fiber after the acid treatment is placed the alkaline solution stir process, then fiber filter, washing, drying are obtained alkaline purification and process fiber, and then fiber is stand-by 80 ℃ of lower oven dry.
Described mineral fibre is sepiolite fibre or fibrous attapulgite; Described acid treating solution is salpeter solution or hydrochloric acid soln, and described acid treating solution amount of substance concentration is 0.1～2mol/L, and acid solution is 8～20 with the fiber quality ratio, and the treatment time is 12～48h.Preferred acid treatment soln amount of substance concentration is 0.5～1mol/L, and acid solution is 12～15 with the fiber quality ratio, and the treatment time is 24h; Described alkaline purification solution is NaOH solution or KOH solution, and alkaline purification solution amount of substance concentration is 0.1～1mol/L, and alkaline solution is 5～10 with the fiber quality ratio, and the treatment time is 0.5～3h.Preferred bases treatment soln amount of substance 0.3～0.5mol/L, alkaline solution is 6～8 with the fiber quality ratio, treatment time 1h; Described mode of washing washs in ethanol 1～3 time for washing in deionized water 1～5 time first again, and wherein washings is 10-30 with the fiber quality ratio.
2) preparation of fiber composite silica wet gel: tetraethoxy, ethanol, nitric acid and water are mixed with silicon sol; Fibre machinery high-speed stirring after the surface treatment is dispersed in the silicon sol, and supersound process disperses to obtain uniform fiber silicon sol suspension again; With the thermal treatment of silicon sol suspension, then in suspension, add ammoniacal liquor, make the gelation of fiber silicon sol suspension, obtain the fiber composite silica wet gel.
Described silicon sol mol ratio is tetraethoxy: ethanol: nitric acid: water=1: 6～16: 1.5 * 10
-3～15 * 10
-3: 2～6; The fiber add-on is 0.1～10% of sol volume, preferred 1～5%; Described fiber dispersion mode is that the fiber after the surface treatment is added in the silicon sol for preparing, and adopts high-speed stirring, and with the speed mechanical dispersion 10-120min of 500-10000r/min, then supersound process is disperseed 10-120min; Fibersol-2 suspension heat treatment mode is at 50～80 ℃ of lower stirring and refluxing 0.5～3h with it; The mol ratio of silicon is 1: 2.7 * 10 in the ammonia vol that adds during the gelation of fiber silicon sol suspension and the colloidal sol
-3～27 * 10
-3
3) aging: as the fiber composite silica wet gel that makes in the step (2) at room temperature to be soaked 12-48h in ethanol, then under 40-80 ℃, in ethanol, soak 12-48h;
4) modification: under 30～80 ℃, place the ethanolic soln of trimethylchlorosilane to soak 12～72h the described fiber composite silica wet gel after aging of step (3);
Preferred modification temperature is 50～60 ℃, and preferred modification time is 24～48h, and the mol ratio of contained silicon-dioxide and trimethylchlorosilane is 0.1～1.0 in the gel, and preferred molar ratio is 0.3～0.5.
5) solvent exchange: place ethanol to carry out solvent exchange the modified fibre composite silicon dioxide wet gel described in the step (4), the quality of each ethanol that adds is 1-5 times of gel quality affects, and time swap is each 12-48h, displacement number of times 2～5 times;
6) drying: take ethanol as the supercritical drying medium, the fiber composite silica wet gel of step (5) gained is carried out supercritical drying process, obtain block fiber-reinforcement silicon dioxide aerogel heat-insulation composite material block.
The aerogel composite of the present invention's preparation is three-dimensional porous network-like structure, and fiber and aerogel matrix phase capacitive are good, and the interface does not have sharp interface in conjunction with firmly; Block aerogel composite density is 0.15～0.25g/cm
3, compressive strength 10% strain energy reaches 0.4～2.0MPa, and thermal conductivity is between 0.016～0.027W/mK.
The wild phase of introducing in the gel molding in integral generally has particle, staple fibre and macrofiber etc.Sepiolite fibre and attapulgite fiber are natural mineral fibers, mainly contain the elements such as Si, Mg, Al, have fibrous porous laminated structure.It is low that they have thermal conductivity, good heat insulating, the characteristics such as thermosteresis is low, and such mineral fibre also has, and intensity is high, nontoxic, pollution-free, oil resistant, alkaline-resisting, corrosion-resistant, can also prevent fires, anti-flaming, strong adhesion, be difficult for the performances such as crack, thereby Chang Zuowei coating lagging material, be widely used in the heat insulation heat preservation energy-saving field.The mineral fibre such as employing sepiolite strengthen aerogel and prepare mechanical property and the heat-proof quality that aerogel heat-insulating material can significantly improve aerogel.
The present invention is based on fiber surface modification technology and sol-gel technique, high with physical strength, thermal conductivity is low, the mineral fibre that thermal stability is good is wild phase, take silicon alkoxide as precursor, adopt the standby fiber composite silica wet gel of soda acid two-step catalysis legal system, obtain block fibre-reinforced aerogel heat-insulation composite material by aging, modification, solvent exchange and supercritical drying again.Acid treatment makes surface modification in the sepiolite, generate the Si-OH active coating, Si-OH at sol-gel process Minerals fiber surface can participate in polycondensation, form the M-O-Si bridged bond with the M-OH dehydrating condensation in the matrix, improve the bonding force of fiber surface and gel-in-matrix, thereby improve the mechanical property of aerogel, acid treatment can also be removed the impurity in the sepiolite duct, play the effect of reaming, be conducive to the duct that more M-OH monomer molecule enters into sepiolite fibre in the colloidal sol dehydration condensation occurs, the number that increases the M-O-Si bridged bond comes the bonding force of fortifying fibre and matrix.Alkaline purification can increase the fiber surface roughness, can further change the surface chemistry state of fiber by alkaline purification, increase fiber surface hydroxyl quantity, alkaline purification can also make the more even of distribution of fiber diameters, can improve fiber composite aerogel material structural uniformity.Fiber after the surface treatment and colloidal sol have good consistency, and between fiber and matrix bonding occur in sol-gel process, make between fiber and matrix in conjunction with more firm.Generally in aerogel, mix wild phase, can increase the thermal conductivity of composite aerogel, but sepiolite fibre and attapulgite fiber are the layered porous structures of a kind of Si of being rich in, Mg and Al, have lower thermal conductivity and good thermostability, so they can obviously not increase its thermal conductivity in the intensity that improves aerogel.
Description of drawings
Fig. 1: strengthen silicon dioxide aerogel heat-insulating composite material sample photo for the present invention prepares sepiolite fibre.
Fig. 2: for the present invention prepares attapulgite fiber-reinforcement silicon dioxide aerogel heat-insulation composite material sample photo.
Fig. 3 (a): for the present invention prepares the scanning electron microscope (SEM) photograph that sepiolite fibre strengthens the silicon dioxide aerogel heat-insulating composite material sample section, magnification is 5000 *, scale is 10 μ m.
Fig. 3 (b): for the present invention prepares the scanning electron microscope (SEM) photograph that sepiolite fibre strengthens fiber in the silicon dioxide aerogel heat-insulating composite material sample, magnification is 45000 *, scale is 1 μ m.
Fig. 4 (a): prepare the scanning electron microscope (SEM) photograph of attapulgite fiber-reinforcement silicon dioxide aerogel heat-insulation composite material sample section for the present invention, magnification is 10000 *, scale is 5 μ m.
Fig. 4 (b): prepare the scanning electron microscope (SEM) photograph of fiber in the attapulgite fiber-reinforcement silicon dioxide aerogel heat-insulation composite material sample for the present invention, magnification is 15000 *, scale is 3 μ m.
Fig. 5 (a): the present invention prepares the transmission electron microscope picture of the used fiber of fiber-reinforcement silicon dioxide aerogel heat-insulation composite material, and scale is 200nm.
Fig. 5 (b): the present invention prepares the transmission electron microscope picture of fiber-reinforcement silicon dioxide aerogel heat-insulation composite material, and scale is 50nm.
Fig. 5 (c): the present invention prepares the transmission electron microscope picture (dark part is fiber, and light-colored part is the aerogel matrix) of fiber and aerogel basal body interface in the fiber-reinforcement silicon dioxide aerogel heat-insulation composite material, and scale is 20nm.
Embodiment
Embodiment 1
Configuration 0.1mol/L salpeter solution is some, is 14 to take by weighing sepiolite fibre by acid solution and fiber quality ratio, load weighted sepiolite fibre is joined in the salpeter solution that configures, and mechanical stirring is processed 12h.Sepiolite suspension after the acid treatment is filtered, the filter cake dispersed with stirring that obtains is washed in distilled water, use distilled water repetitive scrubbing 3 times, use again washing with alcohol 1 time, with the sepiolite fibre oven dry after cleaning; By alkaline solution and fiber quality than being 10 to take by weighing the sepiolite fibre after the acid treatment, load weighted fiber joined in the 1mol/L NaOH solution process 1h, with distilled water repetitive scrubbing 3 times of sepiolite fibre after the alkaline purification, use again washing with alcohol 1 time, the mass ratio of washings and fiber is 15 in described each washing process, and the sepiolite fibre after cleaning is stand-by 80 ℃ of lower oven dry.With tetraethoxy, ethanol, water and 0.15mol/L nital 1: 16: 15 in molar ratio * 10
-3: leave standstill 24h after 4 even mixing and obtain silicon sol, accounting for the silicon sol volume by fiber is 0.1% to take by weighing the fiber after the above-mentioned processing, load weighted fiber is joined in the above-mentioned silicon sol, speed mechanical stirring 10min with 10000r/min, ultra-sonic dispersion 60min obtains fiber silicon sol suspension again, with described suspension at 50 ℃ of lower stirring in water bath backflow 3h.Be 27 * 10 by ammoniacal liquor and silicon sol mol ratio in the above-mentioned suspension again
-3: 1 adds the ammoniacal liquor ethanolic soln of 0.15mol/L, and fiber silicon sol suspension was at 10 minutes inner gels.The fiber composite silica wet gel of gained is soaked 24h at normal temperatures in ethanol, under 40 ℃, in ethanol, soak again 48h.Be 0.1 to measure trimethylchlorosilane by the mol ratio of silicon contained in the wet gel and trimethylchlorosilane, the trimethylchlorosilane that measures with the alcohol dilution liquid that is uniformly mixed, is being soaked 72h with wet gel under 80 ℃ again in above-mentioned mixed solution.Modified fibre composite silicon dioxide wet gel places ethanol to carry out solvent exchange, and the quality of each ethanol that adds is 5 times of gel quality affects, and time swap is each 12h, displacement number of times 2 times; Then carry out supercritical drying, obtain sepiolite fibre and strengthen SiO
2Aerogel composite.
The sepiolite fibre that makes strengthens SiO
2Aerogel composite sample pictorial diagram and stereoscan photograph are shown in accompanying drawing 1, accompanying drawing 3.The aerogel density that obtains is 0.15g/cm
3, compressive strength (10% strain) is 0.4MPa, thermal conductivity is 0.016W/mK.
Embodiment 2
Configuration 2mol/L hydrochloric acid soln is some, is 20 to take by weighing the attapulgite fiber by acid solution and fiber quality ratio, and load weighted attapulgite fiber is joined in the hydrochloric acid soln that configures, and mechanical stirring is processed 36h.Attapulgite suspension after the acid treatment is filtered, the filter cake dispersed with stirring that obtains is washed in distilled water, use distilled water repetitive scrubbing 5 times, use again washing with alcohol twice, with the attapulgite fiber oven dry after cleaning; By alkaline solution and fiber quality than being 8 to take by weighing the sepiolite fibre after the acid treatment, load weighted fiber joined in the 0.1mol/L KOH solution process 0.5h, with distilled water repetitive scrubbing 5 times of attapulgite fiber after the alkaline purification, use again twice of washing with alcohol, the mass ratio of washings and fiber is 10 in described each washing process, and the attapulgite fiber after cleaning is stand-by 80 ℃ of lower oven dry.With tetraethoxy, ethanol, water and 0.15mol/L nital 1: 10: 1.5 in molar ratio * 10
-3: leave standstill 24h after 2 even mixing and obtain silicon sol, be 10% to deserve to be called the fiber of stating after the processing by fiber and silicon sol volume, load weighted fiber is joined in the above-mentioned silicon sol, speed mechanical stirring 120min with 500r/min, ultra-sonic dispersion 10min obtains fiber silicon sol suspension again, with described suspension at 65 ℃ of lower stirring in water bath backflow 1h.Be 2.7 * 10 by ammoniacal liquor and silicon sol mol ratio in the above-mentioned suspension again
-3: 1 adds the ammoniacal liquor ethanolic soln of 0.15mol/L, and fiber silicon sol suspension was at 40 minutes inner gels.The fiber composite silica wet gel of gained is soaked 12h at normal temperatures in ethanol, under 80 ℃, in ethanol, soak again 12h.Be 0.5 to measure trimethylchlorosilane by the mol ratio of silicon contained in the gel and trimethylchlorosilane, the trimethylchlorosilane that measures with the alcohol dilution liquid that is uniformly mixed, is being soaked 24h with wet gel under 50 ℃ again in described mixed solution.Modified fibre composite silicon dioxide wet gel places ethanol to carry out solvent exchange, and the quality of each ethanol that adds is 4 times of gel quality affects, and time swap is each 24h, displacement number of times 3 times; Then carry out supercritical drying, obtain sepiolite fibre and strengthen SiO
2Aerogel composite.
The attapulgite fiber reinforcement SiO that makes
2Aerogel composite pictorial diagram and stereoscan photograph are shown in accompanying drawing 2, accompanying drawing 4.The SiO that obtains
2Aerogel composite density is 0.35g/cm
3, compressive strength (10% strain) is 2.0MPa, thermal conductivity is 0.027W/mK,
Embodiment 3
Configuration 1mol/L salpeter solution is some, is 8 to take by weighing sepiolite fibre by acid solution and fiber quality ratio, load weighted sepiolite fibre is joined in the salpeter solution that configures stir process 48h.Sepiolite suspension after the acid treatment is filtered, the filter cake dispersed with stirring that obtains is washed in distilled water, use distilled water wash 1 time, use again washing with alcohol 3 times.With the sepiolite fibre oven dry after cleaning; By alkaline solution and fiber quality than being 5 to take by weighing the sepiolite fibre after the acid treatment, load weighted fiber joined in the 0.5mol/L NaOH solution process 2h, with distilled water repetitive scrubbing 4 times of sepiolite fibre after the alkaline purification, use again washing with alcohol 3 times, the mass ratio of washings and fiber is 25 in described each washing process, and the sepiolite fibre after cleaning is stand-by 80 ℃ of lower oven dry.With tetraethoxy, ethanol, water and 0.15mol/L nital 1: 6: 8 in molar ratio * 10
-3: leave standstill 24h after 6 even mixing and obtain silicon sol, be 5% to take by weighing the fiber after the above-mentioned processing by fiber and silicon sol volume, load weighted fiber is joined in the above-mentioned silicon sol, speed mechanical stirring 60min with 5000r/min, ultra-sonic dispersion 120min obtains fiber silicon sol suspension again, with described suspension at 80 ℃ of lower stirring in water bath backflow 0.5h.Be 11 * 10 by ammoniacal liquor and silicon sol mol ratio in the above-mentioned suspension again
-3: 1 adds the ammoniacal liquor ethanolic soln of 0.15mol/L, and fiber silicon sol suspension was at 10 minutes inner gels.The fiber composite silica wet gel of gained is soaked 48h at normal temperatures in ethanol, then under 60 ℃, in ethanol, soak 24h.Be 1.0 to measure trimethylchlorosilane by the mol ratio of silicon contained in the gel and trimethylchlorosilane, the trimethylchlorosilane that measures with the alcohol dilution liquid that is uniformly mixed, is being soaked 12h with wet gel under 30 ℃ again in described mixed solution.Modified fibre composite silicon dioxide wet gel places ethanol to carry out solvent exchange, and the quality of each ethanol that adds is 3 times of gel quality affects, and time swap is each 36h, displacement number of times 4 times; Then carry out supercritical drying, obtain sepiolite fibre and strengthen SiO
2Aerogel composite.
The SiO that obtains
2Aerogel composite density is 0.25g/cm
3, compressive strength (10% strain) is 1.2MPa, thermal conductivity is 0.023W/mK.
Embodiment 4
Configuration 0.8mol/L salpeter solution is some, is 12 to take by weighing sepiolite fibre by acid solution and fiber quality ratio, load weighted sepiolite fibre is joined in the salpeter solution that configures stir process 48h.Sepiolite suspension after the acid treatment is filtered, the filter cake dispersed with stirring that obtains is washed in distilled water, use distilled water wash 2 times, use again washing with alcohol 3 times.With the sepiolite fibre oven dry after cleaning; By alkaline solution and fiber quality than being 6 to take by weighing the sepiolite fibre after the acid treatment, load weighted fiber joined in the 0.3mol/L NaOH solution process 3h, with distilled water repetitive scrubbing 2 times of sepiolite fibre after the alkaline purification, use again washing with alcohol 1 time, the mass ratio of washings and fiber is 20 in described each washing process, and the sepiolite fibre after cleaning is stand-by 80 ℃ of lower oven dry.With tetraethoxy, ethanol, water and 0.15mol/L nital 1: 8: 10 in molar ratio * 10
-3: leave standstill 24h after 3 even mixing and obtain silicon sol, be 3% to take by weighing the fiber after the above-mentioned processing by fiber and silicon sol volume, load weighted fiber is joined in the above-mentioned silicon sol, speed mechanical stirring 80min with 3000r/min, ultra-sonic dispersion 30min obtains fiber silicon sol suspension again, with described suspension at 58 ℃ of lower stirring in water bath backflow 2h.Be 14 * 10 by ammoniacal liquor and silicon sol mol ratio in the above-mentioned suspension again
-3: 1 adds the ammoniacal liquor ethanolic soln of 0.15mol/L, and fiber silicon sol suspension was at 10 minutes inner gels.The fiber composite silica wet gel of gained is soaked 36h at normal temperatures in ethanol, then under 50 ℃, in ethanol, soak 36h.Be 0.3 to measure trimethylchlorosilane by the mol ratio of silicon contained in the gel and trimethylchlorosilane, the trimethylchlorosilane that measures with the alcohol dilution liquid that is uniformly mixed, is being soaked 36h with wet gel under 55 ℃ again in described mixed solution.Modified fibre composite silicon dioxide wet gel places ethanol to carry out solvent exchange, and the quality of each ethanol that adds is 1 times of gel quality affects, and time swap is each 48h, displacement number of times 5 times; Then carry out supercritical drying, obtain sepiolite fibre and strengthen SiO
2Aerogel composite.
The SiO that obtains
2Aerogel composite density is 0.21g/cm
-3, compressive strength (10% strain) is 0.9MPa, thermal conductivity is 0.020W/mK.
Configuration 1mol/L salpeter solution is some, is 15 to take by weighing sepiolite fibre by acid solution and fiber quality ratio, load weighted sepiolite fibre is joined in the salpeter solution that configures stir process 24h.Sepiolite suspension after the acid treatment is filtered, the filter cake dispersed with stirring that obtains is washed in distilled water, use distilled water wash 4 times, use again washing with alcohol 3 times.With the sepiolite fibre oven dry after cleaning; By alkaline solution and fiber quality than being 7 to take by weighing the sepiolite fibre after the acid treatment, load weighted fiber joined in the 0.8mol/L NaOH solution process 1.5h, with distilled water repetitive scrubbing 1 time of sepiolite fibre after the alkaline purification, use again twice of washing with alcohol, the mass ratio of washings and fiber is 30 in described each washing process, and the sepiolite fibre after cleaning is stand-by 80 ℃ of lower oven dry.With tetraethoxy, ethanol, water and 0.15mol/L nital 1: 14: 5 in molar ratio * 10
-3: leave standstill 24h after 5 even mixing and obtain silicon sol, be 8% to take by weighing the fiber after the above-mentioned processing by fiber and silicon sol volume, load weighted fiber is joined in the above-mentioned silicon sol, speed mechanical stirring 30min with 8000r/min, ultra-sonic dispersion 80min obtains fiber silicon sol suspension again, with described suspension at 73 ℃ of lower stirring in water bath backflow 1h.Be 9 * 10 by ammoniacal liquor and silicon sol mol ratio in the above-mentioned suspension again
-3: 1 adds the ammoniacal liquor ethanolic soln of 0.15mol/L, and fiber silicon sol suspension was at 10 minutes inner gels.The fiber composite silica wet gel of gained is soaked 48h at normal temperatures in ethanol, then under 70 ℃, in ethanol, soak 24h.Be 0.4 to measure trimethylchlorosilane by the mol ratio of silicon contained in the gel and trimethylchlorosilane, the trimethylchlorosilane that measures with the alcohol dilution liquid that is uniformly mixed, is being soaked 24h with wet gel under 50 ℃ again in described mixed solution.Modified fibre composite silicon dioxide wet gel places ethanol to carry out solvent exchange, and the quality of each ethanol that adds is 2 times of gel quality affects, and time swap is each 48h, displacement number of times 5 times; Then carry out supercritical drying, obtain sepiolite fibre and strengthen SiO
2Aerogel composite.
The SiO that obtains
2Aerogel composite density is 0.22g/cm
-3, compressive strength (10% strain) is 1.0MPa, thermal conductivity is 0.021W/mK.
The present invention proposes silicon dioxide aerogel heat-insulating composite material and preparation method, be described by preferred embodiment, person skilled obviously can be changed or suitably change and combination composition technological method as herein described within not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and the content.
Claims (10)
1. a fiber-reinforcement silicon dioxide aerogel heat-insulation composite material is characterized in that aerogel composite is three-dimensional porous network-like structure, and fiber and aerogel matrix phase capacitive are good, and the interface does not have sharp interface in conjunction with firmly; Block aerogel composite density is 0.15～0.25g/cm
3, compressive strength 10% strain energy reaches 0.4～2.0MPa, and thermal conductivity is at 0.016～0.027W/mK.
2. the preparation method of a kind of fiber-reinforcement silicon dioxide aerogel heat-insulation composite material of claim 1 is characterized in that step is as follows:
1) pre-treatment of fiber: mineral fibre places the acid solution stir process, then fiber filter, washing, drying is obtained acid treated fiber; Fiber after the acid treatment is placed the alkaline solution stir process, then fiber filter, washing, drying are obtained alkaline purification and process fiber, and then fiber is stand-by 80 ℃ of lower oven dry;
2) preparation of fiber composite silica wet gel: tetraethoxy, ethanol, nitric acid and water are mixed with silicon sol; Fibre machinery high-speed stirring after the surface treatment is dispersed in the silicon sol, and supersound process disperses to obtain uniform fiber silicon sol suspension again; With the thermal treatment of silicon sol suspension, then in suspension, add ammoniacal liquor, make the gelation of fiber silicon sol suspension, obtain the fiber composite silica wet gel;
3) aging: as the fiber composite silica wet gel that makes in the step (2) at room temperature to be soaked 12-48h in ethanol, then under 40-80 ℃, in ethanol, soak 12-48h;
4) modification: place the ethanolic soln of trimethylchlorosilane to soak 12～72h under 30～80 ℃ the described fiber composite silica wet gel after aging of step (3), contained silicon-dioxide and the mol ratio of trimethylchlorosilane are 0.1～1.0 in the gel;
5) solvent exchange: place ethanol to carry out solvent exchange the modified fibre composite silicon dioxide wet gel described in the step (4), the quality of each ethanol that adds is 1-5 times of gel quality affects, and time swap is each 12-48h, displacement number of times 2～5 times;
6) drying: take ethanol as the supercritical drying medium, the fiber composite silica wet gel of step (5) gained is carried out supercritical drying process, obtain block fiber-reinforcement silicon dioxide aerogel heat-insulation composite material block.
3. preparation method as claimed in claim 2 is characterized in that the mineral fibre described in the step 1) is sepiolite fibre or fibrous attapulgite.
4. preparation method as claimed in claim 2 is characterized in that acid solution described in the step 1), is salpeter solution or hydrochloric acid soln, and described acid solution amount of substance concentration is 0.1～2mol/L, and acid solution is 8～20 with the fiber quality ratio, and the treatment time is 12～48h.
5. preparation method as claimed in claim 2 is characterized in that alkaline solution described in the step 1) is NaOH solution or KOH solution, and alkaline solution amount of substance concentration is 0.1～1mol/L, and alkaline solution is 5～10 with the fiber quality ratio, and the treatment time is 0.5～3h.
6. preparation method as claimed in claim 2 is characterized in that step 2) described in the silicon sol mol ratio be tetraethoxy: ethanol: nitric acid: water=1: 6～16: 1.5 * 10
-3～15 * 10
-3: 2～6; The fiber add-on is 0.1～10% of sol volume.
7. preparation method as claimed in claim 2, it is characterized in that step 2) in the fiber dispersion mode be that the fiber after the surface treatment is added in the silicon sol prepare, adopt high-speed stirring, with the speed mechanical dispersion 10-120min of 500-10000r/min, then supersound process is disperseed 10-120min; Fibersol-2 suspension heat treatment mode is at 50～80 ℃ of lower stirring and refluxing 0.5～3h with it; The mol ratio of silicon is 1: 2.7 * 10 in the ammonia vol that adds during the gelation of fiber silicon sol suspension and the colloidal sol
-3～27 * 10
-3
8. preparation method as claimed in claim 4 is characterized in that described acid solution amount of substance concentration is 0.5～1mol/L, and acid solution is 12～15 with the fiber quality ratio, and the treatment time is 24h.
9. preparation method as claimed in claim 5 is characterized in that described alkaline solution amount of substance 0.3～0.5mol/L, and alkaline solution is 6～8 with the fiber quality ratio, treatment time 1h.
10. preparation method as claimed in claim 2, it is characterized in that the described fiber composite silica wet gel after aging of step 4) places the ethanolic soln of trimethylchlorosilane to soak 24～48h under 50～60 ℃, contained silicon-dioxide and the mol ratio of trimethylchlorosilane are 0.3～0.5 in the gel.
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|---|---|---|---|
| CN2012104946297A CN103011745A (en) | 2012-11-27 | 2012-11-27 | Silicon-dioxide aerogel heat insulation composite material and preparation method thereof |
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