CN1317187C - Process for preparing stephanoporate powder doped silica aerogel heat-insulation material - Google Patents
Process for preparing stephanoporate powder doped silica aerogel heat-insulation material Download PDFInfo
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- CN1317187C CN1317187C CNB2005100121543A CN200510012154A CN1317187C CN 1317187 C CN1317187 C CN 1317187C CN B2005100121543 A CNB2005100121543 A CN B2005100121543A CN 200510012154 A CN200510012154 A CN 200510012154A CN 1317187 C CN1317187 C CN 1317187C
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Abstract
The present invention provides a preparation method of porous powder doped silica aerogel heat insulating material, which belongs to the technical field of inorganic porous material. The present invention has the following prepared specific technology that porous silicon dioxide powder is prepared by drying in normal pressure; silicon precursor ethyl orthosilicate or methyl orthosilicate hydrolyzes for 2 to 6 hours under the acid condition at the temperature of 50 to 80 DEG C, and a silicon collosol is prepared; fibre, opacifier and porous silica powder are added to the hydrolytic silicon collosol, and added with ammonia to become wet gel; the obtained wet gel ages for 120 to 240 hours in ethanol, wherein the wet gel is exchanged by the ethanol for 3 to 5 times and is dried in a supercritical solvent, so that the silica aerogel heat insulating material is obtained. The present invention has the advantages that the strength of the silica aerogel material is enhanced, the material with good heat insulating performance is simultaneously ensured, and the material prepared by the method has favorable structural compatibility.
Description
Technical field
The invention belongs to the inorganic porous material technical field, a kind of preparation method of stephanoporate powder doped silica aerogel heat-insulation material particularly is provided.Relate in the silica aerogel material and to introduce the intensity that porous silicon-dioxide and/or fiber increase matrix, introduce opalizer strengthen the silica aerogel matrix material in mesophilic range to the barrier effect of infrared light, be a kind of in the preparation method of warm lagging material.
Technical background
Silica aerogel (silica aerogel) is not general traditional foam materials, and it is a kind of nano-porous materials, and the diameter in hole is 1～50nm, and the particle dimension is several nanometers, has three-dimensional network-like structure.Density is very low, and minimum have only 0.03g/cm
3Be three times of air, porosity is up to 99.8%, just because of this, it has little specific refractory power, low Young's modulus, low thermal conductivity, low specific inductivity, high specific surface area, is widely used on heat insulation, sound insulation, chemical industry, electronics, filtration, support of the catalyst.Silica aerogel is the minimum solid material of present known thermal conductivity, thereby as thermal insulation material, is subjected to the extensive attention in each field, and vitreous silica aerogel heat-insulating material has great market in the application of refrigerant latitudes window material.Simultaneously, as thermal insulation material, it has wide practical use in fields such as space flight and military affairs.
Silica aerogel generally prepares by sol-gel method.For guaranteeing that aerogel has enough big void content, the general prepared aerogel monomer material of supercritical drying that adopts is (as document M.J.van Bommel, A.B.deHaan, Journal of Non-Crystalline Solids 186 (1995) 78-82) and A.Venkateswara Raoet al.Materials Research Bulletin 37 (2002) 1667-1677).Silica aerogel is because its bigger porosity and the extremely low solid load that brought thus, thereby shows bigger fragility and extremely low physical strength, and this will greatly limit its practical application.For improving the intensity of silica aerogel, before supercritical drying, wet gel can be carried out burin-in process (M.A.Einarsrud, E.Nilsen, A.Rigacci, G.M.Pajonk, S.Buathier, D.Valette, M.Durant, B.Chevalier, P.Nitz, F.Ehrburger-Dolle, J.Non-cryst.Solids 285 (2001) are 1.); Or introducing fiber or particle (J.Wang, J.Kuhn, X.Lu, Journal of Non-Crystralline Solids 186 (1995) 296-300), effect of extracting by fiber in breaking-down process and fiber or particle consume work of rupture to the deflecting action of crackle, thereby improve the intensity and the toughness of aerogel.But in fiber or particle introducing, the heat-proof quality that will lose aerogel.In addition, this material transmitance to infrared light in the wavelength region of 4-7 μ m is higher, and this will influence the heat-proof quality of material under comparatively high temps, and therefore will introduce some opalizers usually guarantees that aerogel has good heat-proof quality under comparatively high temps.(P.Scheuerpflug?et?al.International?Journal?of?Heat?Mass?andTransfer?28(1985)2299-2306.and?Roland?Caps?et?al.High?Temperatures-HighPressures，15(1983)225-232)。
Summary of the invention
The object of the present invention is to provide a kind of stephanoporate powder doped silica aerogel heat-insulation material preparation method, make in this material homodisperse that porous silica powder and/or inorganic fibre, opalizer are arranged; Realize good structural compatibility, improve the intensity of silica aerogel material.
The present invention introduces the porous silica powder as reinforcer in containing the silica aerogel of opalizer, improve the intensity of silica aerogel material.Because the porous silica powder has higher void content, thereby its adding will can not produce too much influence to the good heat-proof quality of silica aerogel; Identical owing to the porous silica powder simultaneously with the Chemical Composition of silica aerogel matrix, thereby in the supercritical drying process, be easy to form bonding between them, realize good structural compatibility; In addition, the SiO 2 powder that constant pressure and dry forms has higher intensity than the aerogel matrix, thereby in breaking-down process, can realize deflecting action, consume work of rupture, thereby improve the physical strength and the toughness of whole aerogel composite crackle.The concrete technology of preparation is:
A, constant pressure and dry prepare the porous silica powder: water glass, chemical seasoning control agent thorough mixing is even, dropwise add catalyzer and make it into glue, wherein water glass: catalyzer: the mol ratio of chemical seasoning control agent is 1.0: (0.1～2.0): (1.08～5.0).With wet gel in ethanol aging 72～120 hours, then with deionized water wash 3～8 times removing sodium ion, and then in ethanol, wore out 72～120 hours.After dry 8～20 hours at normal temperatures and pressures, drying is 10～20 hours in 110～150 ℃ of loft drier, makes the porous silica powder with wet gel.
B, with 50～80 ℃ of hydrolysis 2～6 hours under acidic conditions of silicon precursor tetraethoxysilance or tetramethoxysilance, preparation silicon sol.
C, the porous silica powder that adds fiber, opalizer and produced by a in the silicon sol of hydrolysis then add ammoniacal liquor again and make it to become wet gel.
D, with the wet gel of gained in ethanol aging 120～240 hours, wherein with ethanol exchange 3～5 times; Dry in supercritical solvent again, obtain silica aerogel heat-insulation material.
Catalyzer of the present invention is 1～2 kind in hydrochloric acid, acetate, the sulfuric acid; Described chemical seasoning control agent is methane amide, dimethyl formamide, in oxalic acid, ethanol, ethylene glycol, the glycerol 1～2 kind; The concentration of chemical seasoning control agent is 1～50 quality %.
The concentration of water glass of the present invention is 5～30 quality %, and the concentration of ammoniacal liquor is 0.1～5 quality %, and the add-on of porous silica powder is 0.1～15 quality %;
Silicon precursor of the present invention is tetraethoxysilance (TEOS) or tetramethoxysilance (TMOS).
The pH value of hydrolysis of the present invention is controlled at 1.5～4.5; The temperature of hydrolysis is 50～80 ℃, and the time of hydrolysis is 2～6 hours.
Fiber of the present invention is that inorganic fibre is 1～2 kind in fiber such as glass fibre, sepiolite, hard Calucium Silicate powder, asbestos or the fibrous material; The diameter of fiber is 0.5～30 micron, and add-on is 0～25 quality %.
Opalizer of the present invention is 1～2 kind in ferric oxide, Z 250, ilmenite, titanium dioxide, chromium sesquioxide, the carbon black; The ratio of opalizer accounts for holosteric 0.1～20 quality %.
The solvent of supercritical drying of the present invention is a kind in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane.
The invention has the advantages that:
1, the preparation of porous silica powder is to be the silicon source with water glass, introduces one or more chemical seasoning control agents simultaneously, prepares by sol-gel, constant pressure and dry.Thereby gained porous silica powder void content height, specific surface area is big, the intensity height, and cost is low.
2, in silica aerogel, introduce the porous silica powder, both increased the monomeric intensity of silica aerogel, guaranteed that again silica aerogel has higher void content and lower thermal conductivity simultaneously, thereby had good heat-proof quality.
The chemical ingredients of the porous silica powder of 3, being introduced is identical with the composition of silica aerogel matrix, thereby can realize the good chemical compatibility and the structural stability of powder and matrix.
4, the adding of opalizer is carried out after silicon precursor carries out prehydrolysis, thereby can prevent the sedimentation of opalizer particulate by the control gelation time, guarantees the microstructural homogeneity of prepared lagging material.
Embodiment
Embodiment 1
Water glass: acetate: methane amide: the mol ratio of ethylene glycol is 1: 0.44: 2: 0.8, and the concentration of water glass is 22 quality %, the concentration of methane amide is 30 quality %; Water glass, methane amide, ethylene glycol thorough mixing is even, dropwise introduce acetate and make it to become gel.Gel was at room temperature worn out 72 hours in the ethanol, wash 5 times to remove Na with tap water
+, use deionized water wash again 3 times, added soaked in absolute ethyl alcohol then 72 hours, put into 110 ℃ dry 12 hours of baking oven under the room temperature after dry 12 hours again, obtain the porous silica powder, its specific surface area is 372cm
2/ g.With TEOS: ethanol: water: hydrochloric acid: the mol ratio of ammoniacal liquor is 1: 8: 3.5: 8.4 * 10
-4: 5.6 * 10
-3Mixing solutions hydrolysis 5 hours under 60 ℃ condition, wherein the concentration of hydrochloric acid is 0.35mol/L.Add above-mentioned porous 2 quality % SiO 2 powders, 2 quality % glass fibre and 10 quality %TiO
2, 5 quality %Fe
2O
3Mix, adding ammoniacal liquor (concentration is 1.5 quality %) then made it to become glue within 5 minutes, in dehydrated alcohol, wore out 120 hours under the room temperature, with dehydrated alcohol exchange 3 times, dry in supercritical co then during this time, the monomer lagging material flawless of gained, thermal conductivity under its room temperature is 0.05W/m.K, and compressive strength is 1.2MPa.
Embodiment 2
Water glass: acetate: methane amide: the mol ratio of ethylene glycol is 1: 0.3: 2.7: 1.0, and the concentration of water glass is 25 quality %, the concentration of methane amide is 18 quality %; Water glass, methane amide, ethylene glycol thorough mixing is even, dropwise introduce acetate and make it to become gel.Gel was at room temperature worn out 120 hours in the ethanol, wash 3 for several times to remove Na with tap water
+, use deionized water wash again 4 times, added soaked in absolute ethyl alcohol then 120 hours, put into 130 ℃ dry 8 hours of baking oven under the room temperature after dry 15 hours again, the specific surface of gained porous silica powder is 350cm
2/ g.With TEOS: ethanol: water: hydrochloric acid: the mol ratio of ammoniacal liquor is 1: 8: 4.5: 8.4 * 10
-4: 5.0 * 10
-3Mixing solutions hydrolysis 3 hours under 70 ℃ condition, wherein the concentration of ammoniacal liquor is 1.5 quality %, the concentration of hydrochloric acid is 0.35mol/L.Add the above-mentioned porous silica powder of 5 quality %, 5 quality % glass fibre and 5 quality %TiO
2, 6 quality %Fe
3O
4, 1 quality %Cr
2O
3, add ammoniacal liquor then and make it within 4 minutes, to become glue, in dehydrated alcohol, wore out 168 hours under the room temperature, during this time with dehydrated alcohol exchange 3 times, dry in Supercritical Ethanol then, the thermal conductivity under the monomer lagging material room temperature of gained is 0.07W/m.K, and compressive strength is 1.5MPa.
Embodiment 3
Water glass: sulfuric acid: methane amide: the mol ratio of ethylene glycol is 1: 0.34: 0.7: 0.38, and the concentration of water glass is 28 quality %, and vitriolic concentration is 0.21mol/L, and the concentration of methane amide is 25 quality %; Water glass, methane amide, ethylene glycol fully stirred it is mixed, dropwise add sulfuric acid then and make it into glue.Gel was at room temperature worn out 72 hours in the ethanol, wash 3 times to remove Na with tap water
+, use deionized water wash again 5 times, added soaked in absolute ethyl alcohol then 72 hours, put into 120 ℃ dry 10 hours of baking oven under the room temperature after dry 12 hours again, the specific surface of the powder of gained silica aerogel is 335cm
2/ g.With TEOS: ethanol: water: the hydrochloric acid mol ratio is 1: 6: 3.5: 8.4 * 10
-4: 5.6 * 10
-3Mixing solutions hydrolysis 1.5 hours under 80 ℃ condition, add 8 above-mentioned quality % voluminous powders, 8 quality % fibers and 15 quality % opalizer TiO
2, 3 quality %Fe
3O
4, 2 quality %Cr
2O
30.5 quality % carbon black, adding ammoniacal liquor (concentration is 1.5 quality %) then made it to become glue within 2 minutes, in dehydrated alcohol, wore out 120 hours under the room temperature, shared during this time dehydrated alcohol exchange 3 times, dry in supercritical co then, the thermal conductivity of the lagging material of gained is 0.08W/m.K, and compressive strength is 1.8MPa.
Claims (6)
1, a kind of stephanoporate powder doped silica aerogel heat-insulation material preparation method, it is characterized in that: the concrete technology of preparation is:
A, constant pressure and dry prepare the porous silica powder: water glass, chemical seasoning control agent thorough mixing is even, dropwise add catalyzer and make it into glue, wherein water glass: catalyzer: the mol ratio of chemical seasoning control agent is 1.0: 0.1～2.0: 1.08～5.0; With wet gel in ethanol aging 72～120 hours, then with deionized water wash 3～8 times removing sodium ion, and then in ethanol, wore out 72～120 hours; After dry 8～20 hours at normal temperatures and pressures, drying is 10～20 hours in 110～150 ℃ of loft drier, makes the porous silica powder with wet gel;
B, with 50～80 ℃ of hydrolysis 2～6 hours under acidic conditions of silicon precursor tetraethoxysilance or tetramethoxysilance, preparation silicon sol;
C, the porous silica powder that adds fiber, opalizer and produced by a in the silicon sol of hydrolysis then add ammoniacal liquor again and make it to become wet gel;
D, with the wet gel of gained in ethanol aging 120～240 hours, wherein with ethanol exchange 3～5 times; Dry in supercritical solvent again, obtain silica aerogel heat-insulation material.
2, in accordance with the method for claim 1, it is characterized in that: described catalyzer is 1～2 kind in hydrochloric acid, acetate, the sulfuric acid; Described chemical seasoning control agent is 1～2 kind in methane amide, dimethyl formamide, oxalic acid, ethanol, ethylene glycol, the glycerol; The concentration of chemical seasoning control agent is 1～50 quality %; The concentration of described water glass is 5～30 quality %, and the concentration of ammoniacal liquor is 0.1～5 quality %, and the add-on of porous silica powder is 0.1～15 quality %.
3, in accordance with the method for claim 1, it is characterized in that: the pH value of described hydrolysis is controlled at 1.5～4.5; The temperature of hydrolysis is 50～80 ℃, and the time of hydrolysis is 2～6 hours.
4, in accordance with the method for claim 1, it is characterized in that: described fiber is 1～2 kind in glass fibre, sepiolite, hard Calucium Silicate powder, the asbestos; The diameter of fiber is 0.5～30 micron, and add-on is 0～25 quality %.
5, in accordance with the method for claim 1, it is characterized in that: described opalizer is 1～2 kind in ferric oxide, Z 250, ilmenite, titanium dioxide, chromium sesquioxide, the carbon black; The ratio of opalizer accounts for holosteric 0.1～20 quality %.
6, in accordance with the method for claim 1, it is characterized in that: the solvent of described supercritical drying is a kind in carbonic acid gas, ethanol, acetone, methyl alcohol, n-propyl alcohol, benzene, butanols, amylalcohol, the octane.
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