CN106592201A - Method for preparing flame retardation-type hydrophobic aerosil composite felt pad under normal pressure - Google Patents

Method for preparing flame retardation-type hydrophobic aerosil composite felt pad under normal pressure Download PDF

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Publication number
CN106592201A
CN106592201A CN201611132217.3A CN201611132217A CN106592201A CN 106592201 A CN106592201 A CN 106592201A CN 201611132217 A CN201611132217 A CN 201611132217A CN 106592201 A CN106592201 A CN 106592201A
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felt pan
solution
solvent
normal pressure
type hydrophobic
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龚伦伦
刘忠
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I Cornaro (beijing) Technology Development Co Ltd
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I Cornaro (beijing) Technology Development Co Ltd
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Abstract

The invention discloses a method for preparing a flame retardation-type hydrophobic aerosil composite felt pad under normal pressure. The method comprises the following steps: S1) uniformly mixing a fire retardant, an infrared barrier and a first solvent, performing ball milling dispersion to obtain a slurry A; S2) uniformly mixing soluble glass and water to obtain a solution B; slowly adding the solution B in an acidic aqueous solution, stirring the solution and stopping addition of the solution B until the pH value is 4-5, then adding the solution B in the slurry A, and uniformly mixing the materials to obtain a sol C; 3) adding the sol C in a mold containing the felt pad, heating the materials to the temperature of 40-70 DEG C, insulating the material to form a gel, adjusting the temperature to 20-60 DEG C, insulating the material and aging the material for 4-8 h to obtain the intermediate felt pad; and S4) performing solvent exchange, silane coupling agent modification and drying processing on the intermediate felt pad to obtain the flame retardation retardation-type hydrophobic aerosil composite felt pad. The retardation-type hydrophobic aerosil composite felt pad has the advantages that cost is low, caking property of aerosil and the felt pad is good, shedding is not easy, and flame resistance is good.

Description

A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel
Technical field
The present invention relates to aerosil technical field, more particularly to a kind of flame retardant type hydrophobic silica aerogel The atmospheric preparation method of compound felt pan.
Background technology
Aerosil is a kind of light nanoporous material, with high porosity, bigger serface, low-density and Low thermal conductivity, these features make silica aerogel material in terms of calorifics, acoustics, optics, microelectronics, particle detection all There is very wide application potential.The subject matter that aerosil is present at present is that preparation cost is too high, is traditionally prepared Aerosil need to adopt supercritical drying process, but supercritical drying needs to use autoclave, complex process, into Originally, high energy consumption, and have certain danger.Therefore constant pressure and dry technique is increasingly becoming everybody focus of attention.But adopt Constant pressure and dry prepares aerosil and can only obtain powder body directly cannot be applied, so having to and other materials is compound With actual application value, wherein aeroge composite fibre felt pan is to apply a kind of most aerogel composites at present.
At present, generally it is combined with fiber felt pan from organic silicon source, but organic silicon source is relatively costly, can increase and produce into This；And needing to carry out that surface is modified or alkylation in the normal pressure preparation technology of aerogel composite, this causes aeroge Contain substantial amounts of organic group in surface, although this causes composite to have hydrophobicity, but also enhances the burning of composite Performance, occurs the phenomenon of heat release and catching fire in hot environment, there is certain potential safety hazard, limits aeroge multiple The popularization and application of composite product；Cost can be greatlyd save from inorganic silicon source, addition fire retardant can increase fire resistance； But the method at present preparing the compound felt pan of aerosil with inorganic silicon source and fiber felt pan is actually rare, and felt pan and Aeroge caking property prepared by inorganic silicon source is not high, and fire resistance is not high, and combustion heat value is higher, should so as to limit its popularization With.
The content of the invention
The technical problem that basic background technology is present, it is multiple that the present invention proposes a kind of flame retardant type hydrophobic silica aerogel The atmospheric preparation method of felt pan is closed, low cost of the present invention, aerosil are good with felt pan caking property, difficult for drop-off, fire-retardant Property is good, and combustion heat value is low.
The present invention proposes a kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, including such as Lower step：
S1, fire retardant, infrared barrier agent and the first solvent are mixed, ball milling dispersion obtains serosity A；
S2, waterglass and water are uniformly mixed so as to obtain into solution B；Solution B is slowly added in acidic aqueous solution, is stirred to pH=4- When 5, stop adding solution B, the serosity A obtained in being subsequently adding S1 to be uniformly mixed so as to obtain colloidal sol C；
S3, the colloidal sol C obtained in S2 is added in the mould containing felt pan, be heated to 40-70 DEG C, be incubated solidifying to being formed Glue, then adjusts the temperature to 20-60 DEG C, is incubated aging 4-8h and obtains middle felt pan；
S4, take S3 in the middle felt pan that obtains carry out solvent exchange, silane coupler modified and dried and obtain fire-retardant Type hydrophobic silica aerogel is combined felt pan.
Preferably, in S1, the mass ratio of fire retardant and the first solvent is 1：5-20, infrared barrier agent and the first solvent Mass ratio is 1：20-200.
Preferably, in S1, fire retardant is halogen-free flame retardants.
Preferably, in S1, fire retardant be APP, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate, ammonium pyrophosphate, Tripolycyanamide, melamine cyanurate, -4 methylol -2,6,7- trioxa -1- phosphabicyclos [2.2.2] octanes of 1- oxygen, phosphoric acid Triphenylmethyl methacrylate, magnesium hydroxide, aluminium hydroxide, basic magnesium carbonate, Basic Magnesium Aluminum Carbonate, antimony oxide, Firebrake ZB, zinc hydroxyl stannate In at least one.
Preferably, in S1, infrared barrier agent be graphite, molybdenum oxide, titanium dioxide, silicon dioxide, in zirconium dioxide It is at least one.
Preferably, in S1, the first solvent is water or ethanol.
Preferably, in S2, during solution B is slowly added in acidic aqueous solution, persistently stir.
Preferably, in S2, it is 2-3.55 that waterglass is modulus, and mass fraction is 32-36wt% sodium silicate aqueous solutions.
Preferably, in S2, waterglass, water, acidic aqueous solution, the volume ratio of serosity A are 1：2-6：0.25-0.5：0.1- 1。
Preferably, in S2, in acidic aqueous solution, the concentration of solute is 6-12mol/L.
Preferably, in S2, acidic aqueous solution is that aqueous hydrochloric acid solution, aqueous sulfuric acid, aqueous solution of nitric acid or phosphoric acid are water-soluble Liquid, preferably aqueous hydrochloric acid solution.
Preferably, in S3, in normal pressure or subnormal ambient, the colloidal sol C obtained in S2 is added into the mould containing felt pan In.
Preferably, in S3, in vacuum environment, the colloidal sol C obtained in S2 is added in the mould containing felt pan.
Preferably, in S3, heated with heater.
Preferably, in S3, with baking oven, microwave or heating in water bath.
Preferably, in S3, the material of felt pan is glass fibre, ceramic fibre, rock wool, at least one in mineral wool.
Preferably, in S3, the material of mould is glass, nylon or politef.
Preferably, in the solvent exchange procedure of S4, the middle felt pan for obtaining is added in the second solvent, temperature is adjusted in S3 Spend to 40-60 DEG C, insulation solvent exchange 2-3 time, every time insulation solvent exchange 6-8h, the middle felt pan after taking-up process is added In 3rd solvent, 40-60 DEG C is adjusted the temperature to, insulation solvent exchange 2-3 time is incubated solvent exchange 6-8h every time, and taking-up is obtained Middle felt pan after solvent exchange.
Preferably, the second solvent is methanol, ethanol, acetone, ethylene glycol, at least one in isopropanol.
Preferably, the 3rd solvent is normal hexane, hexamethylene or normal heptane.
Preferably, S4 it is silane coupler modified during, by solvent exchange after middle felt pan add the 3rd solvent In, adding silane coupler to mix, be warming up to 40-60 DEG C, be incubated 12-24h, taking-up obtains the modified middle felt pan in surface.
Preferably, S4 it is silane coupler modified during, silane coupler be trim,ethylchlorosilane, two silicon of hexamethyl Azane, hexamethyl disiloxane or APTES.
Preferably, S4 it is silane coupler modified during, silane coupler with middle felt pan Si atoms mole Than for 0.3-0.85：1.
Preferably, in S4, it is dried and is dried or is vacuum dried for normal pressure classification.
Preferably, in S4, being dried and drying being classified for normal pressure, the dry process of normal pressure classification is incubated to be warming up to 60 DEG C 2h, is warming up to 120 DEG C, is incubated 2h, is warming up to 150 DEG C, is incubated 4h.
Above-mentioned water be deionized water or tap water in one kind.
In above-mentioned S3, normal pressure is a normal atmosphere, and negative pressure is the gas pressure state less than normal pressure, negative pressure state bag Include vacuum state.
In above-mentioned S3, do not specify the consumption of colloidal sol C and felt pan, its consumption is determined according to concrete operations.
Above-mentioned solvent exchange, it is silane coupler modified during, the second solvent, the 3rd solvent, the 4th solvent are with submergence Between felt pan for best, do not specify the addition of solvent, determine its addition according to concrete operations.
The present invention is raw material from cheap waterglass, cheap and easy to get, can greatly save cost；By fire retardant and infrared barrier Agent is prepared into serosity after ball milling dispersion so as to can be uniformly dispersed in colloidal sol, can avoid adding fire retardant, infrared barrier The problem for causing aerosil combustion heat value to increase after agent, in addition homodisperse halogen-free flame retardants, infrared barrier agent Cooperate composition flame-retardant system with aerosil, while fire resistance of the present invention being increased, make guarantor of the present invention Relatively low combustion heat value is held, noninflammability of the present invention is capable of achieving and can be reached A level standards；The present invention has fire retardant and red by dispersed The colloidal sol C of outer barrier, in adding the mould containing felt pan, and makes silicon dioxide gas by being thermally formed gel, burin-in process Gel is combined closely with felt pan so as to difficult for drop-off, so as to increased the fire resistance of felt pan；It is silane coupler modified to increased The hydrophobic performance of the present invention, so as to obtain, with low cost, good flame resistance, combustion heat value be low, aerosil is difficult for drop-off Compound felt pan.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, fire retardant, infrared barrier agent and the first solvent are mixed, ball milling dispersion obtains serosity A；
S2, waterglass and water are uniformly mixed so as to obtain into solution B；Solution B is slowly added in acidic aqueous solution, is stirred to pH= When 4.5, stop adding solution B, the serosity A obtained in being subsequently adding S1 to be uniformly mixed so as to obtain colloidal sol C；
S3, by the colloidal sol C obtained in S2 add the mould containing felt pan in, be heated to 55 DEG C, be incubated to formed gel, so After adjust the temperature to 40 DEG C, be incubated aging 6h and obtain middle felt pan；
S4, take S3 in the middle felt pan that obtains carry out solvent exchange, silane coupler modified and dried and obtain fire-retardant Type hydrophobic silica aerogel is combined felt pan.
Embodiment 2
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, fire retardant, infrared barrier agent and water are mixed, ball milling dispersion obtains serosity A, wherein, the matter of fire retardant and water Amount is than being 1：5, infrared barrier agent is 1 with the mass ratio of water：200, fire retardant is ammonium dihydrogen phosphate, triphenyl phosphate, hydroxide The mixture of aluminum composition, infrared barrier agent are graphite, the mixture of zirconium dioxide composition；
S2, it is 2 by modulus, mass fraction is that 36wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；Solution B is delayed During slow addition concentration is for the aqueous solution of nitric acid of 6mol/L, when stirring to pH=4, stop adding solution B, obtain in being subsequently adding S1 Serosity A be uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, HNO3Aqueous solution, the volume ratio of serosity A are 1：6：0.25： 1；
S3, in atmospheric pressure environment, by the colloidal sol C obtained in S2 add the mould containing felt pan in, be heated to heater 40 DEG C, it is incubated to gel is formed, then adjusts the temperature to 60 DEG C, is incubated aging 4h and obtains middle felt pan, wherein, the material of felt pan For the mixed materials that ceramic fibre and rock wool constitute；
S4, take S3 in the middle felt pan that obtains carry out solvent exchange, silane coupler modified and dried and obtain fire-retardant Type hydrophobic silica aerogel is combined felt pan.
Embodiment 3
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, by melamine cyanurate, molybdenum oxide and ethanol mix, ball milling dispersion obtain serosity A, wherein, cyanuric acid three Poly cyanamid is 1 with the mass ratio of ethanol：20, molybdenum oxide is 1 with the mass ratio of ethanol：20；
S2, it is 3.55 by modulus, mass fraction is that 32wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；By solution B It is slowly added to, in the aqueous sulfuric acid that concentration is 12mol/L, when stirring to pH=5, stop adding solution B, be subsequently adding in S1 The serosity A for obtaining is uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, H2SO4Aqueous solution, the volume ratio of serosity A are 1：2： 0.5：0.1；
S3, in subnormal ambient, by the colloidal sol C obtained in S2 add the mould containing ceramic fibre felt pan in, use baking oven 70 DEG C are heated to, are incubated to gel is formed, are then adjusted the temperature to 20 DEG C, be incubated aging 8h and obtain middle felt pan；
S4, take S3 in during the middle felt pan that obtains adds methanol, adjust the temperature to 40 DEG C, insulation solvent exchange 3 times, every time Insulation solvent exchange 6h, the middle felt pan after taking-up process, in adding hexamethylene, adjusts the temperature to 60 DEG C, is incubated solvent exchange 2 Secondary, insulation solvent exchange 8h, takes out the middle felt pan after obtaining solvent exchange every time；Middle felt pan after by solvent exchange is added In hexamethylene, add hexamethyl disiloxane to mix, be warming up to 40 DEG C, be incubated 24h, taking-up obtains the modified middle felt in surface Pad；Surface modified middle felt pan vacuum drying is obtained into the compound felt pan of flame retardant type hydrophobic silica aerogel, wherein, six Tetramethyldisiloxane is 0.3 with the mol ratio of Si atoms in middle felt pan：1.
Embodiment 4
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, fire retardant, infrared barrier agent and ethanol are mixed, ball milling dispersion obtains serosity A, wherein, fire retardant and ethanol Mass ratio be 1：10, infrared barrier agent is 1 with the mass ratio of ethanol：150, fire retardant is triphenyl phosphate, magnesium hydroxide, boron The mixture of sour zinc composition, infrared barrier agent are molybdenum oxide, titanium dioxide, the mixture of silicon dioxide composition；
S2, it is 2.5 by modulus, mass fraction is that 35wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；By solution B It is slowly added in the phosphate aqueous solution that concentration is 8mol/L, when stirring to pH=4.2, stop adding solution B, be subsequently adding S1 In the serosity A that obtains be uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, phosphate aqueous solution, the volume ratio of serosity A are 1： 5：0.35：0.7；
S3, in vacuum environment, by the colloidal sol C obtained in S2 add the mould containing felt pan in, heating in water bath to 50 DEG C, It is incubated to gel is formed, then adjusts the temperature to 50 DEG C, is incubated aging 5h and obtains middle felt pan, wherein, the material of felt pan is glass Glass fiber, ceramic fibre, the mixed materials of mineral wool composition；
S4, take S3 in during the middle felt pan that obtains adds the mixed solvent of ethylene glycol and isopropanol composition, adjust the temperature to 60 DEG C, insulation solvent exchange 2 times, insulation solvent exchange 8h, the middle felt pan after taking-up process, in adding normal heptane, adjust every time To 40 DEG C, insulation solvent exchange 3 times is incubated solvent exchange 6h to section temperature every time, and taking-up obtains the middle felt pan after solvent exchange； During middle felt pan after by solvent exchange adds normal heptane, add APTES to mix, be warming up to 60 DEG C, Insulation 12h, taking-up obtain the modified middle felt pan in surface；Surface modified middle felt pad is warming up to into 60 DEG C, 2h is incubated, 120 DEG C are warming up to, 2h are incubated, are warming up to 150 DEG C, insulation 4h obtains the compound felt pan of flame retardant type hydrophobic silica aerogel, its In, APTES is 0.85 with the mol ratio of Si atoms in middle felt pan：1.
Embodiment 5
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, by melamine cyanurate, zirconium dioxide and water mix, ball milling dispersion obtain serosity A, wherein, cyanuric acid three Poly cyanamid is 1 with the mass ratio of water：15, zirconium dioxide is 1 with the mass ratio of water：100；
S2, it is 3 by modulus, mass fraction is that 33wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；Solution B is delayed During slow addition concentration is for the aqueous hydrochloric acid solution of 10mol/L, when stirring to pH=4.8, stop adding solution B, be subsequently adding in S1 The serosity A for obtaining is uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, HCl/water solution, the volume ratio of serosity A are 1：3： 0.4：0.3；
S3, in atmospheric pressure environment, by the colloidal sol C obtained in S2 add the mould containing ceramic fibre felt pan in, microwave adds Heat is incubated to gel is formed, then adjusts the temperature to 30 DEG C to 60 DEG C, is incubated aging 7h and is obtained middle felt pan；
S4, take S3 in during the middle felt pan that obtains adds isopropanol, adjust the temperature to 50 DEG C, insulation solvent exchange 3 times, often Secondary insulation solvent exchange 8h, the middle felt pan after taking-up process, in adding normal hexane, adjust the temperature to 50 DEG C, and insulation solvent is handed over Change 3 times, every time insulation solvent exchange 8h, taking-up obtains the middle felt pan after solvent exchange；Middle felt pan after by solvent exchange In adding hexamethylene, add trim,ethylchlorosilane to mix, be warming up to 50 DEG C, be incubated 18h, taking-up obtains the modified centre in surface Felt pan；Surface modified middle felt pan vacuum drying is obtained into the compound felt pan of flame retardant type hydrophobic silica aerogel, wherein, Trim,ethylchlorosilane is 0.63 with the mol ratio of Si atoms in middle felt pan：1.
Embodiment 6
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, APP, titanium dioxide and water are mixed, ball milling dispersion obtains serosity A, wherein, APP and water Mass ratio is 1：10, titanium dioxide is 1 with the mass ratio of water：90；
S2, it is 3.55 by modulus, mass fraction is that 34wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；By solution B It is slowly added to, in the aqueous hydrochloric acid solution that concentration is 12mol/L, when stirring to pH=4.5, stop adding solution B, be subsequently adding S1 In the serosity A that obtains be uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, HCl/water solution, the volume ratio of serosity A are 1： 3.4：0.25：0.44；
S3, in atmospheric pressure environment, by the colloidal sol C obtained in S2 add the mould containing glass fiber mat in, baking oven adds Heat is incubated to gel is formed, then adjusts temperature 45 C to 60 DEG C, is incubated aging 4h and is obtained middle felt pan, wherein, glass fibre The specification of felt pan is 100mm × 100mm × 6mm；
S4, take S3 in during the middle felt pan that obtains adds ethanol, adjust the temperature to 45 DEG C, insulation solvent exchange 3 times, every time Insulation solvent exchange 6h, the middle felt pan after taking-up process, in adding normal hexane, adjusts the temperature to 45 DEG C, is incubated solvent exchange 2 Secondary, insulation solvent exchange 8h, takes out the middle felt pan after obtaining solvent exchange every time；Middle felt pan after by solvent exchange is added In normal hexane, add trim,ethylchlorosilane to mix, be warming up to 45 DEG C, be incubated 8h, taking-up obtains the modified middle felt pan in surface； Surface modified middle felt pad is warming up to into 60 DEG C, 12h is incubated, is warming up to 120 DEG C, be incubated 2h, be warming up to 150 DEG C, be incubated 4h obtains the compound felt pan of flame retardant type hydrophobic silica aerogel, wherein, Si atoms in trim,ethylchlorosilane and middle felt pan Mol ratio is 0.6：1.
Embodiment 7
A kind of atmospheric preparation method of the compound felt pan of flame retardant type hydrophobic silica aerogel, comprises the steps：
S1, aluminium hydroxide, titanium dioxide and water are mixed, ball milling dispersion obtains serosity A, wherein, aluminium hydroxide and water Mass ratio is 1：10, titanium dioxide is 1 with the mass ratio of water：90；
S2, it is 3 by modulus, mass fraction is that 34wt% sodium silicate aqueous solutions and water are uniformly mixed so as to obtain solution B；Solution B is delayed Slowly in concentration being added for the aqueous hydrochloric acid solution of 6mol/L, when stirring to pH=4.5, stop adding solution B, obtain in being subsequently adding S1 To serosity A be uniformly mixed so as to obtain colloidal sol C, wherein, sodium silicate aqueous solution, water, HCl/water solution, serosity A volume ratio be 1：3.4： 0.5：0.44；
S3, in atmospheric pressure environment, by the colloidal sol C obtained in S2 add the mould containing glass fiber mat in, microwave adds Heat is incubated to gel is formed, then adjusts the temperature to 60 DEG C to 60 DEG C, is incubated aging 4h and is obtained middle felt pan, wherein, glass fibers The specification of dimension felt pan is 100mm × 100mm × 6mm；
S4, take S3 in during the middle felt pan that obtains adds acetone, adjust the temperature to 45 DEG C, insulation solvent exchange 3 times, every time Insulation solvent exchange 6h, the middle felt pan after taking-up process, in adding normal hexane, adjusts the temperature to 45 DEG C, is incubated solvent exchange 2 Secondary, insulation solvent exchange 8h, takes out the middle felt pan after obtaining solvent exchange every time；Middle felt pan after by solvent exchange is added In normal hexane, add hexamethyldisiloxane to mix, be warming up to 45 DEG C, be incubated 8h, taking-up obtains the modified middle felt in surface Pad；Surface modified middle felt pad is warming up to into 60 DEG C, 24h is incubated, is warming up to 120 DEG C, be incubated 2h, be warming up to 150 DEG C, protected Warm 4h obtains the compound felt pan of flame retardant type hydrophobic silica aerogel, wherein, hexamethyldisiloxane is former with Si in middle felt pan The mol ratio of son is 0.4：1.
Performance detection is carried out to embodiment 2-7, it is as a result as follows：
Project Density g/cm3 Heat conductivity w/ (mK) Contact angle ° Combustion heat value J/g
Embodiment 2 0.159 0.249 162 2411
Embodiment 3 0.161 0.251 164 2394
Embodiment 4 0.165 0.250 163 2357
Embodiment 5 0.143 0.242 163 2468
Embodiment 6 0.156 0.024 161 2400
Embodiment 7 0.170 0.025 160 2300
As can be seen from the above table, combustion heat value of the present invention is low, and heat conductivity is little.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.

Claims (10)

1. a kind of flame retardant type hydrophobic silica aerogel is combined the atmospheric preparation method of felt pan, it is characterised in that including as follows Step：
S1, fire retardant, infrared barrier agent and the first solvent are mixed, ball milling dispersion obtains serosity A；
S2, waterglass and water are uniformly mixed so as to obtain into solution B；Solution B is slowly added in acidic aqueous solution, when stirring to pH=4-5, Stop adding solution B, the serosity A obtained in being subsequently adding S1 to be uniformly mixed so as to obtain colloidal sol C；
S3, by the colloidal sol C obtained in S2 add the mould containing felt pan in, be heated to 40-70 DEG C, be incubated to formed gel, so After adjust the temperature to 20-60 DEG C, be incubated aging 4-8h and obtain middle felt pan；
S4, take S3 in the middle felt pan that obtains carry out solvent exchange, silane coupler modified and dried and obtain flame retardant type dredging Water aerosil is combined felt pan.
2. flame retardant type hydrophobic silica aerogel is combined the atmospheric preparation method of felt pan, its feature according to claim 1 It is that, in S1, the mass ratio of fire retardant and the first solvent is 1：5-20, infrared barrier agent are 1 with the mass ratio of the first solvent： 20-200。
3. flame retardant type hydrophobic silica aerogel according to claim 1 or claim 2 is combined the atmospheric preparation method of felt pan, and which is special Levy and be, in S1, fire retardant is halogen-free flame retardants.
4. according to any one of claim 1-3, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that in S1, fire retardant be APP, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate, ammonium pyrophosphate, Tripolycyanamide, melamine cyanurate, -4 methylol -2,6,7- trioxa -1- phosphabicyclos [2.2.2] octanes of 1- oxygen, phosphoric acid Triphenylmethyl methacrylate, magnesium hydroxide, aluminium hydroxide, basic magnesium carbonate, Basic Magnesium Aluminum Carbonate, antimony oxide, Firebrake ZB, zinc hydroxyl stannate In at least one.
5. according to any one of claim 1-4, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that in S1, infrared barrier agent be graphite, molybdenum oxide, titanium dioxide, silicon dioxide, in zirconium dioxide extremely Few one kind.
6. according to any one of claim 1-5, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that in S1, the first solvent are water or ethanol.
7. according to any one of claim 1-6, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that in S2, during solution B is slowly added in acidic aqueous solution, persistently stirs；Preferably, in S2 In, it is 2-3.55 that waterglass is modulus, and mass fraction is 32-36wt% sodium silicate aqueous solutions；Preferably, in S2, waterglass, Water, acidic aqueous solution, the volume ratio of serosity A are 1：2-6：0.25-0.5：0.1-1；Preferably, in S2, in acidic aqueous solution The concentration of solute is 6-12mol/L；Preferably, in S2, acidic aqueous solution is aqueous hydrochloric acid solution, aqueous sulfuric acid, nitric acid aqueous solution Solution or phosphate aqueous solution, preferably aqueous hydrochloric acid solution.
8. according to any one of claim 1-7, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan The colloidal sol C obtained in S2, in normal pressure or subnormal ambient, is added the mould containing felt pan by method, it is characterised in that in S3 In；Preferably, in S3, in vacuum environment, the colloidal sol C obtained in S2 is added in the mould containing felt pan；Preferably, exist In S3, heated with heater；Preferably, in S3, with baking oven, microwave or heating in water bath；Preferably, in S3, the material of felt pan Matter is glass fibre, ceramic fibre, rock wool, at least one in mineral wool；Preferably, in S3, the material of mould is glass, Buddhist nun Dragon, or politef.
9. according to any one of claim 1-8, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that in the solvent exchange procedure of S4, the middle felt pan for obtaining is added in the second solvent, temperature is adjusted in S3 Spend to 40-60 DEG C, insulation solvent exchange 2-3 time, every time insulation solvent exchange 6-8h, the middle felt pan after taking-up process is added In 3rd solvent, 40-60 DEG C is adjusted the temperature to, insulation solvent exchange 2-3 time is incubated solvent exchange 6-8h every time, and taking-up is obtained Middle felt pan after solvent exchange；Preferably, the second solvent be methanol, ethanol, acetone, ethylene glycol, in isopropanol at least one Kind；Preferably, the 3rd solvent is normal hexane, hexamethylene or normal heptane.
10. according to any one of claim 1-9, flame retardant type hydrophobic silica aerogel is combined the normal pressure preparation side of felt pan Method, it is characterised in that S4 it is silane coupler modified during, by solvent exchange after middle felt pan add the 3rd solvent In, adding silane coupler to mix, be warming up to 40-60 DEG C, be incubated 12-24h, taking-up obtains the modified middle felt pan in surface； Preferably, S4 it is silane coupler modified during, silane coupler be trim,ethylchlorosilane, hexamethyldisiloxane, six Tetramethyldisiloxane or APTES；Preferably, S4 it is silane coupler modified during, silane idol Connection agent is 0.3-0.85 with the mol ratio of Si atoms in middle felt pan：1；Preferably, in S4, be dried for normal pressure classification be dried or Vacuum drying；Preferably, in S4, being dried and drying being classified for normal pressure, the dry process of normal pressure classification is incubated to be warming up to 60 DEG C 2h, is warming up to 120 DEG C, is incubated 2h, is warming up to 150 DEG C, is incubated 4h.
CN201611132217.3A 2016-12-09 2016-12-09 Method for preparing flame retardation-type hydrophobic aerosil composite felt pad under normal pressure Pending CN106592201A (en)

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CN107541929A (en) * 2017-08-30 2018-01-05 湖南天欣科技股份有限公司 A kind of preparation method of hydrophobic fiber enhancing alumina aerogels
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CN108314411A (en) * 2018-01-03 2018-07-24 深圳中凝科技有限公司 The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine
CN108584964A (en) * 2018-05-15 2018-09-28 天津摩根坤德高新科技发展有限公司 A kind of environment-friendly type aeroge modification heat-insulating fireproof material formula and processing technology
CN111099876A (en) * 2019-12-20 2020-05-05 山东工业陶瓷研究设计院有限公司 Preparation method of low-cost silicon dioxide aerogel composite flexible heat insulation material
TWI741746B (en) * 2020-08-20 2021-10-01 趙國昇 Manufacturing method of silica aerogel composite fiber blanket
CN114045151A (en) * 2021-11-26 2022-02-15 广州市白云化工实业有限公司 Flame-retardant silicone sealant and preparation method thereof
CN115349382A (en) * 2022-08-24 2022-11-18 青岛沃纳精工科技有限公司 Fire-retardant green house heat preservation quilt
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CN115785704A (en) * 2022-12-01 2023-03-14 华阳新材料科技集团有限公司 Preparation method of coal ash-based non-expansion type steel structure fireproof heat-insulation coating

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Application publication date: 20170426