CN113563049A - Hydrophobic silica aerogel composite material with high thermal stability and low calorific value and preparation method thereof - Google Patents
Hydrophobic silica aerogel composite material with high thermal stability and low calorific value and preparation method thereof Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
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Abstract
The invention belongs to the technical field of heat-insulating composite materials, and provides a hydrophobic silica aerogel composite material with high thermal stability and low calorific value and a preparation method thereof. According to the invention, an inorganic silicon source is used as a precursor, and the hydrophobic gel is obtained through gelation and modification; then, soaking the matrix material in hydrophobic gel to obtain a pretreated composite material; when an organic silicon source is taken as a precursor, adding a matrix material in the gelation process to ensure that the matrix material fully adsorbs silicon source hydrolysate; sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to obtain a pretreated composite material; and then carrying out heat treatment on the pretreated composite material to orderly reduce the number of methyl groups on the surface of the silicon dioxide aerogel, reduce residual organic liquid on the surface and in pores of the silicon dioxide aerogel and optimize the microscopic morphology of the silicon dioxide aerogel, so that the final composite material has high thermal stability and low combustion heat value.
Description
Technical Field
The invention relates to the technical field of heat-insulating composite materials, in particular to a hydrophobic silica aerogel composite material with high thermal stability and low calorific value and a preparation method thereof.
Background
The silica aerogel has a typical three-dimensional nano-porous network structure and has extremely low density (approximately equal to 3 kg/m)3) Extremely low thermal conductivity (less than or equal to 0.016W/(m.k)), and high specific surface area (more than or equal to 800 m)2In terms of/g). The extremely low thermal conductivity of the silicon dioxide aerogel enables the silicon dioxide aerogel to have great application space and market in the field of heat preservation and insulation. In addition, most silica aerogels are fragile, have poor molding and the like, so the silica aerogels in the market mainly take powder and blocky particles as main components.
The powdery silicon dioxide aerogel is compounded with the functional material to obtain the composite material with the silicon dioxide performance and the functional material performance, so that the silicon dioxide aerogel has wider application prospect in the fields of pipeline heat preservation, building internal and external wall heat preservation, space suit, air transportation and the like. For example, chinese patent publication No. CN106587908A provides a method for preparing a high temperature resistant hydrophobic silica aerogel heat insulation felt, and the related data indicate that the method does not greatly improve the thermal stability and combustion performance of the silica aerogel composite material.
Therefore, how to improve the thermal stability and combustibility of silica aerogel composite materials becomes a critical issue to be solved in the industry.
Disclosure of Invention
In view of the above, the present invention aims to provide a hydrophobic silica aerogel composite material with high thermal stability and low calorific value and a preparation method thereof. The silica aerogel composite material prepared by the preparation method provided by the invention has excellent thermal stability and combustibility.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which comprises the following steps:
sequentially adding an alcohol solvent, a hydrophobic modifier and an acid catalyst into the inorganic silicon source wet gel to carry out first hydrophobic modification to obtain hydrophobic silica wet gel;
dipping a base material into the hydrophobic silica wet gel to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
Preferably, the temperature of the first hydrophobic modification is 35-85 ℃, and the time is 2-12 h.
The invention also provides a preparation method of the hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which comprises the following steps:
mixing the organic silicon source hydrolysate with a base material, and performing gelation to obtain a gel composite system;
sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to obtain an alkane gel composite system;
mixing the alkane gel composite system and a hydrophobic modifier, and carrying out second hydrophobic modification to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
Preferably, the pH value of the gelation is 6.5-7.5, the temperature is 20-60 ℃, and the time is 1-12 h.
Preferably, the temperature of the second hydrophobic modification is 30-60 ℃, and the time is 2-24 h.
Preferably, the hydrophobic modifier is a monomethyl hydrophobic modifier, a dimethyl hydrophobic modifier, a trimethyl hydrophobic modifier, or a hexamethyl hydrophobic modifier;
the monomethyl hydrophobic modifier comprises one or more of methyltrichlorosilane, methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-octyltriethoxysilane, and 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane;
the dimethyl hydrophobic modifier comprises one or more of dimethyl dichlorosilane, dimethyl dimethoxysilane, dimethyl diethoxysilane, diethyl dimethoxysilane and diethyl diethoxysilane;
the trimethyl hydrophobic modifier comprises trimethyl chlorosilane;
the hexamethyl hydrophobic modifier comprises one or more of hexamethyldisiloxane, hexamethyldisilazane, and hexamethyldisilazane.
Preferably, the base material comprises one or more of an inorganic polymer insulation board, a wood fiber board, a rock wool board, a glass wool board, a composite magnesium aluminum silicate insulation material, a foam glass insulation board, a fiber reinforced composite insulation board, a ceramic fiber board, a gold board and a glass fiber felt.
Preferably, the heat treatment comprises: and heating to the heat treatment temperature for heat preservation, wherein the heat treatment temperature is 200-1000 ℃, the heating rate is 1-20 ℃/min, and the heat preservation time is 5-1440 min.
Preferably, when the hydrophobic modifier is a monomethyl hydrophobic modifier, the heat treatment temperature is preferably 500-600 ℃, and the heat preservation time is preferably 30-960 min;
when the hydrophobic modifier is a dimethyl hydrophobic modifier, the heat treatment temperature is preferably 600-700 ℃, and the heat preservation time is preferably 30-960 min;
when the hydrophobic modifier is a trimethyl hydrophobic modifier, the heat treatment temperature is preferably 700-800 ℃, and the heat preservation time is preferably 30-960 min;
when the hydrophobic modifier is a hexamethyl hydrophobic modifier, the heat treatment temperature is preferably 700-800 ℃, and the heat preservation time is preferably 30-960 min.
The invention also provides the hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which is prepared by the preparation method of the technical scheme.
The invention provides a preparation method of a hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which comprises the following steps: sequentially adding an alcohol solvent, a hydrophobic modifier and an acid catalyst into the inorganic silicon source wet gel to carry out first hydrophobic modification to obtain hydrophobic silica wet gel; dipping a base material into the hydrophobic silica wet gel to obtain a pretreated composite material; and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value. Adding an alcohol solvent, a hydrophobic modifier and an acidic catalyst into inorganic silicon source wet gel to perform first hydrophobic modification, endowing the silica wet gel with hydrophobicity, then soaking a base material into the obtained hydrophobic silica wet gel, and soaking the hydrophobic silica wet gel into the base material to enable the base material to fully absorb the hydrophobic silica wet gel; and then carrying out heat treatment on the pretreated composite material, wherein the heat treatment can orderly reduce the number of methyl groups on the surface of the silicon dioxide aerogel, reduce residual organic liquid on the surface and in pores, and optimize the microscopic morphology of the silicon dioxide aerogel, so that the final silicon dioxide aerogel composite material has high thermal stability and low combustion heat value.
The invention also provides another preparation method of the hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which comprises the following steps: mixing the organic silicon source hydrolysate with a base material, and performing gelation to obtain a gel composite system; sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to obtain an alkane gel composite system; mixing the alkane gel composite system and a hydrophobic modifier, and carrying out second hydrophobic modification to obtain a pretreated composite material; and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value. The organic silicon source hydrolysate is mixed with the matrix material, so that the matrix material fully adsorbs the organic silicon source hydrolysate; sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to ensure that all water in the gel composite system is replaced by alkane; and then heat treatment is carried out, so that the number of methyl groups on the surface of the silicon dioxide aerogel can be orderly reduced, residual organic liquid on the surface and in pores of the silicon dioxide aerogel is reduced, and the microscopic morphology of the silicon dioxide aerogel is optimized, so that the final silicon dioxide aerogel composite material has high thermal stability and low combustion heat value.
Detailed Description
The invention provides a preparation method of a hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which comprises the following steps:
sequentially adding an alcohol solvent, a hydrophobic modifier and an acid catalyst into the inorganic silicon source wet gel to carry out first hydrophobic modification to obtain hydrophobic silica wet gel;
dipping a base material into the hydrophobic silica wet gel to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
In the invention, an alcohol solvent, a hydrophobic modifier and an acidic catalyst are sequentially added into an inorganic silicon source wet gel to carry out first hydrophobic modification, so as to obtain hydrophobic silica wet gel.
In the present invention, the preparation method of the inorganic silicon source wet gel preferably comprises the following steps: and mixing the inorganic silicon source and water, and gelling to obtain the inorganic silicon source wet gel.
In the present invention, the inorganic silicon source preferably includes one or more of sodium silicate, potassium silicate, lithium silicate, and rice hull ash; the inorganic silicon source is preferably used in the form of an inorganic silicon source solution, the modulus of the inorganic silicon source solution is preferably a commercially available conventional form, specifically, the modulus of the sodium silicate solution is preferably 2.4 to 3.3, the modulus of the potassium silicate solution is preferably 2.4 to 3.3, and the modulus of the lithium silicate solution is preferably 2 to 4.9. In the present invention, the volume ratio of the inorganic silicon source solution to water is preferably 1: 3. in the present invention, the water is preferably deionized water.
In the invention, in the process of preparing the inorganic silicon source wet gel, the gelation temperature is preferably 15-30 ℃, and the time is preferably 1-24 h; the gelation is preferably performed under a condition of standing. In the invention, in the process of preparing the inorganic silicon source wet gel, the pH value of the gelation is preferably 3.5-4.5, and more preferably 4; the pH of the gelation is preferably achieved by addition of an acid solution; the acid solution preferably comprises an inorganic acid and/or an organic acid; the inorganic acid preferably comprises one or more of hydrochloric acid, hypochlorous acid, perchloric acid, sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid, sulfurous acid, nitrous acid, hydrosulfuric acid, hydroiodic acid, and hydrobromic acid; the organic acid preferably comprises one or more of oxalic acid, acetic acid, oxalic acid, pyruvic acid, lactic acid, benzoic acid, acrylic acid, propionic acid and oleic acid; the concentration and the addition amount of the acid solution are not particularly limited, and the pH value of gelation can be 3.5 to 4.5.
In the present invention, the inorganic silicon source wet gel is preferably crushed before being mixed with the alcohol solvent, and the parameters of the crushing are not particularly limited in the present invention.
In the present invention, the alcohol solvent preferably includes one or more of monohydric alcohol, dihydric alcohol and trihydric alcohol; the monohydric alcohol preferably comprises one or more of methanol, ethanol, propanol, isopropanol, butanol, isobutanol, and diacetone alcohol; the dihydric alcohol preferably comprises one or more of ethylene glycol, propylene glycol, diethylene glycol, butylene glycol and diethylene glycol; the triol preferably comprises glycerol.
In the present invention, the hydrophobic modifier is preferably a monomethyl hydrophobic modifier, a dimethyl hydrophobic modifier, a trimethyl hydrophobic modifier, or a hexamethyl hydrophobic modifier. In the present invention, the monomethyl hydrophobic modifier preferably comprises one or more of methyltrichlorosilane, methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-octyltriethoxysilane, and 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane. In the present invention, the dimethyl hydrophobic modifier preferably comprises one or more of dimethyldichlorosilane, dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane and diethyldiethoxysilane. In the present invention, the trimethyl hydrophobic modifier preferably comprises trimethyl chlorosilane. In the present invention, the hexamethyl hydrophobic modifier preferably comprises one or more of hexamethyldisiloxane, hexamethyldisilazane, and hexamethyldisilazane.
In the present invention, the acidic catalyst preferably comprises an inorganic acid, and the inorganic acid preferably comprises one or more of phosphoric acid, concentrated hydrochloric acid, perchloric acid, hydroiodic acid, hydrobromic acid, and concentrated sulfuric acid. In the present invention, the phosphoric acid is preferably present at a mass concentration of 85%.
In the invention, the volume ratio of the inorganic silicon source solution, the alcohol solvent, the hydrophobic modifier and the acidic catalyst in the preparation raw material of the inorganic silicon source wet gel is preferably (20-25): (20-25): (40-60): (2-10).
In the invention, after the alcohol solvent is added, the mixture is preferably stirred for 1-6 min. In the invention, after the hydrophobic modifier is added, the mixture is preferably stirred for 2-10 min.
In the invention, the temperature of the first hydrophobic modification is preferably 35-85 ℃, and the time is preferably 2-12 h. In the present invention, the first hydrophobic modification is preferably performed under the condition of a water bath.
After the hydrophobic silica wet gel is obtained, the invention soaks the matrix material in the hydrophobic silica wet gel to obtain the pretreated composite material.
In the invention, the base material preferably comprises an inorganic polymer insulation board, a wood fiber board, a rock wool board, a glass wool board, a composite magnesium aluminum silicate insulation material, a foam glass insulation board and a fiber reinforced composite materialOne or more of the heat insulation board, the ceramic fiber board, the real metal board and the glass fiber felt, and the glass fiber felt is further preferable. In the present invention, the size of the glass fiber mat is preferably 100 x 40 x 1.5 mm; the density of the glass fiber mat is preferably 0.14-0.19 g/cm3. In the present invention, since the silica aerogel is very brittle and fragile; the matrix material can compensate for this disadvantage of silica aerogel; and the use of the hydrophobic modifier can endow the composite material with hydrophobicity.
After the pretreated composite material is obtained, the pretreated composite material is sequentially dried and thermally treated under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
In the present invention, the protective atmosphere preferably includes one or more of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, and carbon monoxide, and more preferably argon.
In the invention, the drying temperature is preferably 100-150 ℃, and the drying time is preferably 1-4 h.
In the present invention, the heat treatment preferably includes: and raising the temperature to the heat treatment temperature for heat preservation, wherein the heat treatment temperature is preferably 200-1000 ℃, the temperature raising rate is preferably 1-20 ℃/min, and the heat preservation time is preferably 5-1440 min.
In the invention, when the hydrophobic modifier is a monomethyl hydrophobic modifier, the heat treatment temperature is preferably 500-600 ℃, and the heat preservation time is preferably 30-960 min.
In the invention, when the hydrophobic modifier is a dimethyl hydrophobic modifier, the heat treatment temperature is preferably 600-700 ℃, and the heat preservation time is preferably 30-960 min.
In the invention, when the hydrophobic modifier is a trimethyl hydrophobic modifier, the heat treatment temperature is preferably 700-800 ℃, and the heat preservation time is preferably 30-960 min.
In the invention, when the hydrophobic modifier is a hexamethyl hydrophobic modifier, the heat treatment temperature is preferably 700-800 ℃, and the heat preservation time is preferably 30-960 min.
The invention also provides another preparation method of the silicon dioxide aerogel composite material, which comprises the following steps:
mixing the organic silicon source hydrolysate with the matrix material, and performing gelation to obtain a gel composite system;
sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to obtain an alkane gel composite system;
mixing the alkane gel composite system and a hydrophobic modifier, and carrying out second hydrophobic modification to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
The invention mixes the organic silicon source hydrolysate with the matrix material for gelation to obtain the gel composite system.
In the present invention, the preparation method of the organic silicon source hydrolysate preferably comprises the following steps:
and mixing the organic silicon source, an alcohol solvent and water, and hydrolyzing to obtain the organic silicon source hydrolysate.
In the present invention, the organic silicon source preferably includes one or more of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), tetrabutyl orthosilicate, methyltrimethoxysilane (MTMS), Methyltriethoxysilane (MTES), Ethyltrimethoxysilane (ETMS), ethyltriethoxysilane (ETES), dimethyldimethoxysilane (DMDMS), dimethyldiethoxysilane (DMDES), diethyldimethoxysilane (DEDMS), polysiloxane, 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane (EDAS), and n-octyltriethoxysilane. In the present invention, the polysiloxane preferably includes Polydimethylsiloxane (PDMS) and/or Polydiethylsiloxane (PDES).
In the present invention, the kind of the alcohol solvent is preferably the same as that of the alcohol solvent described in the above technical scheme, and is not described herein again.
In the present invention, the water is preferably deionized water.
In the invention, the volume ratio of the organic silicon source to the alcohol solvent is preferably (5-6): (15-20).
In the present invention, the mixing of the silicon source, the alcohol solvent and the water is preferably performed under a stirring condition, and the stirring time is preferably 5 to 30 min.
In the invention, the hydrolysis temperature is preferably 30-60 ℃; the time is preferably 3-12 h. In the invention, the pH value of the hydrolysis is preferably 4.5-6.0; the pH value of the hydrolysis is preferably realized by adding acid liquor, the type of the acid liquor is preferably consistent with that of the acid liquor in the technical scheme, and the description is omitted, and the concentration and the addition amount of the acid liquor are not specifically limited, so long as the pH value of the hydrolysis is 4.5-6.0.
In the present invention, the kind of the base material is preferably the same as that of the base material described in the above technical solution, and is not described herein again.
In the invention, when the gel composite system is prepared, the gelation temperature is preferably 20-60 ℃, and the time is preferably 1-12 h. In the invention, the pH value of the gelation is preferably 6.5-7.5; the pH of the gelation is preferably achieved by adding an alkaline agent, which preferably comprises an inorganic base and/or an organic base. In the present invention, the inorganic base preferably includes one or more of ammonia, sodium hydroxide, ammonium fluoride, ammonium hydrogen carbonate, sodium carbonate and sodium hydrogen carbonate. In the present invention, the organic base preferably includes ethanolamine, diethanolamine, triethanolamine, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, propylamine, dipropylamine, tripropylamine, isopropylamine, diisopropylamine, 1, 2-dimethylpropylamine, 1, 2-propylenediamine, 2-propyleneamine, cyclopropylamine, N-butylamine, di-N-butylamine, isobutylamine, sec-butylamine, 1, 4-butylenediamine, diisobutylamine, hexylamine, 2-ethylhexylamine, hexamethylenediamine, monoethanolamine, diethanolamine, triethanolamine, 3-propanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, N-methyldiethanolamine, N-diethylethanolamine, triethylenediamine, diethylenetriamine, hexamethylenetetramine, hexamethyleneimine, triethylenediamine, One or more of cyclic ethylene imine, morpholine, piperazine, cyclohexylamine, aniline, diphenylamine, benzidine, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, o-toluidine, m-toluidine, p-toluidine, 2, 3-dimethylaniline, 1-naphthylamine, 2-naphthylamine and naphthyldiamine. The amount of the alkaline agent used is not particularly limited, and the pH for gelation may be 6.5 to 7.5.
After the gel composite system is obtained, the gel composite system is subjected to alcohol displacement and alkane displacement in sequence to obtain the alkane gel composite system.
In the present invention, the alcohol-substitution reagent is preferably ethanol, and the ethanol is preferably absolute ethanol. In the invention, the number of times of alcohol replacement is preferably 1-6, and the time of each alcohol replacement is preferably 2-12 h.
In the present invention, the alkane-displacing agent is preferably a n-alkane; the n-alkanes preferably include one or more of n-hexane, n-heptane, n-octane, cyclohexane, n-dodecane, and n-hexadecane. In the invention, the alkane replacement frequency is preferably 1-6, and the time of each alkane replacement is preferably 2-12 h.
In the invention, the water in the gel composite system can be replaced by the normal alkane through alcohol replacement and alkane replacement, and the normal alkane is a low surface tension solvent, so that the shrinkage rate in the drying process can be reduced and the skeleton collapse can be reduced.
After the alkane gel composite system is obtained, the alkane gel composite system and the hydrophobic modifier are mixed for second hydrophobic modification, and the pretreated composite material is obtained.
In the present invention, the kind of the hydrophobic modifier is preferably the same as that of the hydrophobic modifier described in the above technical solution, and is not described herein again. In the present invention, the hydrophobic modifier is preferably used in the form of a solution of the hydrophobic modifier; the solvent in the hydrophobic modifier solution is preferably an alkane-displacing agent. In the invention, the volume percentage of the hydrophobic modifier in the second hydrophobic modified system is preferably 1-20%.
In the invention, the temperature of the second hydrophobic modification is preferably 30-60 ℃, and the time is preferably 2-24 h.
After the pretreated composite material is obtained, the pretreated composite material is placed in a protective atmosphere to be dried and subjected to heat treatment in sequence, and the hydrophobic silica aerogel composite material with high thermal stability and low calorific value is obtained.
In the present invention, the kind of the protective atmosphere, the drying condition and the heat treatment condition are preferably the same as those in the above technical solution, and are not described herein again.
The invention also provides the hydrophobic silica aerogel composite material with high thermal stability and low calorific value, which is prepared by the preparation method of the technical scheme. The silicon dioxide aerogel composite material provided by the invention has excellent thermal stability and combustion performance, and also has excellent hydrophobicity.
The high thermal stability, low calorific value hydrophobic silica aerogel composite and the method for preparing the same according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Comparative example 1
Water glass (modulus 2.4) and deionized water at a ratio of 1: 3, taking 50mL of diluted water glass, adding phosphoric acid while stirring to adjust the pH value to 4 to initiate gelation, and then standing and aging for 9h at normal temperature. The aged gel was crushed, 50mL of ethanol was added to the gel, followed by mechanical stirring for 2min, and 100mL of Hexamethyldisiloxane (HMDSO) was added thereto, and mechanical stirring was continued for 5 min. And then putting the sol into a magnetic stirring water bath, carrying out magnetic stirring at the rotating speed of 600rpm in the water bath at the temperature of 65 ℃, adding 20mL of phosphoric acid (the mass concentration is 85%) during stirring, and obtaining the hydrophobic silica wet gel after 4 hours. Immersing a glass fiber felt (with the size of 100 multiplied by 40 multiplied by 1.5mm) into the hydrophobic silica wet gel, and obtaining a pretreated composite material after the glass fiber felt fully absorbs the hydrophobic silica wet gel; and (3) putting the pretreated composite material into a drying oven, and drying for 4 hours at the temperature of 120 ℃ under the air condition to obtain the hydrophobic silicon dioxide aerogel composite material.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3The heat conductivity is 35.4 mW/(m.k) based on a transient hot wire method, the contact angle is 143 degrees, the total combustion heat value (GCV) is 3.7MJ/kg based on an oxygen bomb calorimeter, and the heat release rate peak value (T) is measured by a differential scanning calorimeterpeak) Is 336 ℃.
Example 1
Example 1 was prepared according to the same procedure as comparative example 1. After the pretreated composite material is obtained, the pretreated composite material is placed into a tubular furnace filled with argon, and the temperature is kept at 120 ℃ for 4 hours to obtain the hydrophobic silica aerogel composite material. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 250 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.18g/cm3Thermal conductivity of 35.6 mW/(m.k), contact angle of 143 degrees, total heat of combustion (GCV) of 3.6MJ/kg, heat release rate peak value (T)peak) The temperature was 507 ℃.
Example 2
Example 2 was prepared according to the same procedure as in comparative example 1. After the pretreated composite material is obtained, putting the pretreated composite material into a tubular furnace filled with argon, and preserving the heat for 4 hours at the temperature of 120 ℃ to obtain the hydrophobic silica aerogel composite material. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.24g/cm3The heat conductivity is 41.2 mW/(m.k), the contact angle is 133 degrees, the total combustion heat value (GCV) is 3.2MJ/kg, and the heat release rate peak value (T)peak) The temperature was 620 ℃.
Example 3
Example 3 was prepared according to the same procedure as in comparative example 1. After the pretreated composite material is obtained, putting the pretreated composite material into a tubular furnace filled with nitrogen, and preserving heat for 4 hours at the temperature of 120 ℃ to obtain the hydrophobic silica aerogel composite material. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.24g/cm3The heat conductivity is 41.4 mW/(m.k), the contact angle is 134 degrees, the total combustion heat value (GCV) is 3.2MJ/kg, and the heat release rate peak value (T)peak) It was 617 ℃.
Example 4
Example 4 was prepared according to the same procedure as in comparative example 1. After the pretreated composite material is obtained, the pretreated composite material is placed into a tubular furnace filled with helium, and heat preservation is carried out for 4 hours at the temperature of 120 ℃ to obtain the hydrophobic silica aerogel composite material. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.25g/cm3The heat conductivity is 41.8 mW/(m.k), the contact angle is 135 degrees, the total combustion heat value (GCV) is 3.2MJ/kg, and the heat release rate peak value (T)peak) At 623 ℃.
Example 5
Example 5 was prepared according to the same procedure as in comparative example 1. After the pretreated composite material is obtained, putting the pretreated composite material into a tubular furnace filled with neon, and preserving heat for 4 hours at the temperature of 120 ℃ to obtain the hydrophobic silica aerogel composite material. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.24g/cm3The heat conductivity is 41.5 mW/(m.k), the contact angle is 134 degrees, the total combustion heat value (GCV) is 3.2MJ/kg, and the heat release rate peak value (T)peak) It was 621 ℃.
Comparative examples 1 to 5 and comparative example 1 can find that: the HMDSO modified hydrophobic silica aerogel composite material still maintains high hydrophobicity and low thermal conductivity after being subjected to heat treatment at 700 ℃ for 2h in different inert gas atmospheres, but the high thermal stability of the HMDSO modified hydrophobic silica aerogel composite material is improved to 620 ℃ compared with that of the non-heat-treated hydrophobic silica aerogel composite material, and the combustion heat value is reduced by 10%. This shows that the hydrophobic silica aerogel composite material prepared by the method maintains high hydrophobicity and low thermal conductivity, the high thermal stability is greatly improved, and the thermal hazard is effectively reduced.
Comparative example 2
Tetraethyl orthosilicate (TEOS), absolute ethyl alcohol (EtOH), deionized water (DI. H)2O) according to a volume ratio of 5: 15: 1, dripping a proper amount of 0.1M hydrochloric acid to enable the pH value to be 5.5, stirring for 5min, and then putting the solution into a water bath kettle at the temperature of 45 ℃ for hydrolysis for 12h to obtain hydrolysate. And (3) taking out the hydrolysate, adding a proper amount of 0.5M ammonia water to enable the pH value to be 6.5, stirring for 3min, standing the gel at normal temperature, immersing a glass fiber felt (with the size of 100 multiplied by 40 multiplied by 1.5mm) into the sol before the gel occurs (the gel occurs for 30min), and aging for 4h to obtain a gel composite system. Adding a proper amount of absolute ethyl alcohol into the gel composite system to replace pore water in the wet gel, and exchanging for 12 hours; then, the absolute ethyl alcohol is poured out, a proper amount of absolute ethyl alcohol is added into the absolute ethyl alcohol, the exchange is continued for 12 hours, and the absolute ethyl alcohol is exchanged for 2 times in 24 hours. Then pouring out absolute ethyl alcohol, adding a proper amount of n-hexane to exchange the absolute ethyl alcohol in the wet gel for 12 hours, repeating n-hexane exchange once again, exchanging n-hexane for 2 times in 24 hours, and obtaining an alkane gel composite system after finishing solvent exchange; adding proper amount of Trimethylchlorosilane (TMCS)/n-hexane with the concentration of 12% into the alkane gel composite system for mixingAnd putting the solution into a water bath kettle at 45 ℃ for hydrophobic modification for 12 hours to obtain the pretreated composite material. And (3) putting the pretreated composite material into a drying oven, and drying for 4 hours at the temperature of 120 ℃ under the air condition to obtain the hydrophobic silicon dioxide aerogel composite material.
The specific parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.16g/cm3The heat conductivity is 34.9 mW/(m.k), the contact angle is 142 degrees, the total combustion heat value (GCV) is 3.71MJ/kg, and the heat release rate peak value (T)peak) It was 274 ℃.
Example 6
Example 6 the same as the earlier preparation procedure of comparative example 2, the pretreated composite was placed in a tube furnace filled with argon and the temperature was maintained at 120 ℃ for 4h to obtain a hydrophobic silica aerogel composite. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 350 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3Thermal conductivity of 35.2 mW/(m.k), contact angle of 143 degrees, total heat of combustion (GCV) of 3.53MJ/kg, heat release rate peak value (T)peak) It was 305 ℃.
Example 7
Example 7 the same as the earlier preparation procedure of comparative example 2, the pretreated composite was placed in a tube furnace filled with argon and held at 120 ℃ for 4h to obtain a hydrophobic silica aerogel composite. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3Thermal conductivity of 35.2 mW/(m.k), contact angle of 143 degrees, total heat of combustion (GCV) of 3.53MJ/kg, heat release rate peak value (T)peak) It was 585 ℃.
Example 8
Example 8 the same as the earlier preparation procedure of comparative example 2, the pretreated composite was placed in a tubular furnace with nitrogen and held at 120 ℃ for 4h to obtain a hydrophobic silica aerogel composite. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3Thermal conductivity of 35.5 mW/(m.k), contact angle of 140 degrees, total heat of combustion (GCV) of 3.5MJ/kg, heat release rate peak value (T)peak) 591 ℃ is obtained.
Example 9
Example 9 the same as the earlier preparation procedure of comparative example 2, the pretreated composite was placed in a tube furnace filled with helium and held at 120 ℃ for 4h to obtain a hydrophobic silica aerogel composite. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3Thermal conductivity of 35.2 mW/(m.k), contact angle of 142 degrees, total heat of combustion (GCV) of 3.5MJ/kg, heat release rate peak value (T)peak) At 587 ℃.
Example 10
Example 10 the same as the earlier preparation procedure of comparative example 2, the pretreated composite was placed in a tubular furnace with neon gas and held at 120 ℃ for 4h to obtain a hydrophobic silica aerogel composite. And continuously placing the hydrophobic silica aerogel composite material in a tubular furnace, raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel composite material with high thermal stability and low combustion heat value.
The performance parameters of the obtained composite material are as follows: the size is 100 multiplied by 40 multiplied by 1.5mm, the density is 0.17g/cm3Thermal conductivity of 35.3 mW/(m.k), contact angle of 142 degrees, total heat of combustion (GCV) of 3.5MJ/kg, heat release rate peak value (T)peak) Is 590 ℃.
Comparative examples 6 to 10 and comparative example 2 can find that: the TMCS modified hydrophobic silica aerogel composite material still keeps high hydrophobicity and low thermal conductivity after being subjected to heat treatment at 700 ℃ for 2 hours in different inert gas atmospheres, but the thermal stability of the TMCS modified hydrophobic silica aerogel composite material is improved by nearly 300 ℃ compared with that of the non-heat-treated hydrophobic silica aerogel composite material, and the combustion heat value is reduced by 10%. The hydrophobic silica aerogel composite material prepared by the invention maintains high hydrophobicity and low thermal conductivity, greatly improves the thermal stability and effectively reduces the thermal hazard.
Comparative example 3
Commercially available hydrophobic silica aerogel blankets. The relevant parameters are as follows: the size is 100 multiplied by 40 multiplied by 3mm, the density is 0.2g/cm3Thermal conductivity of 22.3 mW/(m.k), contact angle of 139 degrees, total heat of combustion (GCV) of 3.5MJ/kg, heat release rate peak value (T)peak) Is 336 ℃.
Example 11
Example 11 is the same as the commercial hydrophobic silica aerogel blanket of comparative example 3. Putting the hydrophobic silica aerogel felt into a tubular furnace filled with argon, preserving the heat for 4 hours at the temperature of 100-120 ℃, then increasing the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to finally obtain the hydrophobic silica aerogel felt with high thermal stability and low combustion heat value.
The performance parameters of the obtained aerogel felt are as follows: the size is 100 multiplied by 40 multiplied by 3mm, the density is 0.24g/cm3Thermal conductivity of 27.2 mW/(m.k), contact angle of 135 degrees, total heat of combustion (GCV) of 2.9MJ/kg, heat release rate peak value (T)peak) It was 617 ℃.
Example 12
Example 12 is the same as the commercial hydrophobic silica aerogel blanket of comparative example 3. Putting the hydrophobic silica aerogel felt into a tube furnace filled with nitrogen, preserving heat for 4 hours at the temperature of 100-120 ℃, then increasing the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to finally obtain the hydrophobic silica aerogel felt with high thermal stability and low combustion heat value.
The performance parameters of the obtained aerogel felt are as follows: the size is 100 multiplied by 40 multiplied by 3mm, the density is 0.24g/cm3Thermal conductivity of 27.1 mW/(m.k), contact angle of 132 degrees, total heat of combustion (GCV) of 2.9MJ/kg, heat release rate peak value (T)peak) At 623 ℃.
Example 13
Example 13 is the same as the commercial hydrophobic silica aerogel blanket of comparative example 3. Putting the hydrophobic silica aerogel felt into a tubular furnace filled with helium, preserving heat for 4 hours at the temperature of 100-120 ℃, then increasing the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to finally obtain the hydrophobic silica aerogel felt with high thermal stability and low combustion heat value.
The performance parameters of the obtained aerogel felt are as follows: the size is 100 multiplied by 40 multiplied by 3mm, the density is 0.24g/cm3Thermal conductivity of 27.5 mW/(m.k), contact angle of 133 degrees, total heat of combustion value (GCV) of 2.9MJ/kg, heat release rate peak value (T)peak) The temperature was 615 ℃.
Example 14
Example 14 is the same as the commercial hydrophobic silica aerogel blanket of comparative example 3. Putting the hydrophobic silica aerogel felt into a tubular furnace filled with neon, preserving heat for 4 hours at the temperature of 100-120 ℃, then raising the temperature to 700 ℃ at the heating rate of 10 ℃/min, and carrying out heat treatment for 2 hours to obtain the hydrophobic silica aerogel felt with high thermal stability and low combustion heat value.
The performance parameters of the obtained aerogel felt are as follows: the size is 100 multiplied by 40 multiplied by 3mm, the density is 0.24g/cm3The heat conductivity is 27.1 mW/(m.k), the contact angle is 139 degrees, the total combustion heat value (GCV) is 2.9MJ/kg, and the heat release rate peak value (T)peak) It was 621 ℃.
Comparative examples 11 to 14 and comparative example 3 can find that: the commercial hydrophobic silica aerogel felt still maintains high hydrophobicity and low thermal conductivity after being subjected to heat treatment at 700 ℃ for 2 hours under different inert gas atmospheres, but the thermal stability of the hydrophobic silica aerogel felt is improved by nearly one time compared with that of the hydrophobic silica aerogel felt which is not subjected to heat treatment, and the combustion heat value is also reduced by 17%. The heat treatment method has the same good effect on the commercial hydrophobic silica aerogel felt, and the heat stability of the heat treatment method is greatly improved and the heat hazard of the heat treatment method is effectively reduced while the high hydrophobicity and the low thermal conductivity of the heat treatment method are maintained.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a hydrophobic silica aerogel composite material with high thermal stability and low calorific value comprises the following steps:
sequentially adding an alcohol solvent, a hydrophobic modifier and an acid catalyst into the inorganic silicon source wet gel to carry out first hydrophobic modification to obtain hydrophobic silica wet gel;
dipping a base material into the hydrophobic silica wet gel to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
2. The preparation method of claim 1, wherein the temperature of the first hydrophobic modification is 35-85 ℃ and the time is 2-12 h.
3. A preparation method of a hydrophobic silica aerogel composite material with high thermal stability and low calorific value comprises the following steps:
mixing the organic silicon source hydrolysate with the matrix material, and performing gelation to obtain a gel composite system;
sequentially carrying out alcohol replacement and alkane replacement on the gel composite system to obtain an alkane gel composite system;
mixing the alkane gel composite system and a hydrophobic modifier, and carrying out second hydrophobic modification to obtain a pretreated composite material;
and sequentially drying and thermally treating the pretreated composite material under a protective atmosphere to obtain the hydrophobic silica aerogel composite material with high thermal stability and low calorific value.
4. The method according to claim 3, wherein the gelation time is 1 to 12 hours at a pH of 6.5 to 7.5 and a temperature of 20 to 60 ℃.
5. The preparation method according to claim 3, wherein the temperature of the second hydrophobic modification is 30-60 ℃ and the time is 2-24 h.
6. The production method according to claim 1 or 3, characterized in that the hydrophobic modifier is a monomethyl hydrophobic modifier, a dimethyl hydrophobic modifier, a trimethyl hydrophobic modifier, or a hexamethyl hydrophobic modifier;
the monomethyl hydrophobic modifier comprises one or more of methyltrichlorosilane, methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-octyltriethoxysilane, and 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane;
the dimethyl hydrophobic modifier comprises one or more of dimethyl dichlorosilane, dimethyl dimethoxysilane, dimethyl diethoxysilane, diethyl dimethoxysilane and diethyl diethoxysilane;
the trimethyl hydrophobic modifier comprises trimethyl chlorosilane;
the hexamethyl hydrophobic modifier comprises one or more of hexamethyldisiloxane, hexamethyldisilazane, and hexamethyldisilazane.
7. The method of claim 1 or 3, wherein the base material comprises one or more of an inorganic polymer insulation board, a wood wool board, a rock wool board, a glass wool board, a composite magnesium aluminum silicate insulation material, a foam glass insulation board, a fiber reinforced composite insulation board, a ceramic fiber board, a real gold board, and a glass fiber mat.
8. The production method according to claim 1 or 3, characterized in that the heat treatment comprises: and heating to the heat treatment temperature for heat preservation, wherein the heat treatment temperature is 200-1000 ℃, the heating rate is 1-20 ℃/min, and the heat preservation time is 5-1440 min.
9. The method of claim 8, wherein:
when the hydrophobic modifier is a monomethyl hydrophobic modifier, the heat treatment temperature is 500-600 ℃, and the heat preservation time is 30-960 min;
when the hydrophobic modifier is a dimethyl hydrophobic modifier, the heat treatment temperature is 600-700 ℃, and the heat preservation time is 30-960 min;
when the hydrophobic modifier is a trimethyl hydrophobic modifier, the heat treatment temperature is 700-800 ℃, and the heat preservation time is 30-960 min;
when the hydrophobic modifier is a hexamethyl hydrophobic modifier, the heat treatment temperature is 700-800 ℃, and the heat preservation time is 30-960 min.
10. A high thermal stability, low calorific value hydrophobic silica aerogel composite obtainable by the process of any one of claims 1 to 9.
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