CN106753437A - A kind of low heat value silicon dioxide silica aerogel composite material and preparation method thereof - Google Patents

A kind of low heat value silicon dioxide silica aerogel composite material and preparation method thereof Download PDF

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Publication number
CN106753437A
CN106753437A CN201611132215.4A CN201611132215A CN106753437A CN 106753437 A CN106753437 A CN 106753437A CN 201611132215 A CN201611132215 A CN 201611132215A CN 106753437 A CN106753437 A CN 106753437A
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heat value
ball
silicon dioxide
low heat
silica aerogel
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马丽艳
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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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/02Inorganic materials
    • C09K21/04Inorganic materials containing phosphorus
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/06Organic materials
    • C09K21/10Organic materials containing nitrogen

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

The invention discloses a kind of low heat value silicon dioxide silica aerogel composite material, its raw material includes by weight:50 90 parts of aerosil, 5 40 parts of halogen-free flame retardants, 1 10 parts of inorganic nano fire retarding synergist, 0.1 2 parts of opacifier, 0.1 0.5 parts of dispersant, 0.2 0.6 parts of lubricant, 15 parts of reinforcing agent.The invention also discloses the preparation method of above-mentioned low heat value silicon dioxide silica aerogel composite material, comprise the following steps:Each raw material is uniformly mixed so as to obtain material A;By in abrading-ball and material A addition ball grinder, dispersion solvent is added, with the speed of 100 300r/min after sealing, the 10h of ball milling 6 takes out abrading-ball, is warming up to 60 120 DEG C, is dried to obtain low heat value silicon dioxide silica aerogel composite material.Good flame resistance of the present invention, combustion heat value is low.

Description

A kind of low heat value silicon dioxide silica aerogel composite material and preparation method thereof
Technical field
It is compound the present invention relates to aerosil technical field, more particularly to a kind of low heat value aerosil Material and preparation method thereof.
Background technology
Heat preserving and insulating material application on building materials has turned into focus of concern in recent years.Silica airsetting Glue turns into a kind of new and effective heat preserving and insulating material because of its extremely low thermal conductivity factor.Aeroge in civilian insulation material especially Exterior-wall heat insulation aspect, compared to the tradition such as the organic materials such as traditional polystyrene, polyurethane and foam cement, expanded perlite Inorganic insulation material, does not decompose, the low advantage of thermal conductivity factor with non-ignitable, high temperature, is greatly improved heat-insulating property and reduces Security against fire hidden danger.Further, since the high porosity of aerosil so that dielectric constant in static air very It is close, therefore aerosil has outstanding wave transparent performance.
But silica aerogel material also shows some drawbacks in application process.Because silica airsetting The modified link of surface hydrophobicity in glue preparation process, introduces flammable alkyl organic group in the structure, is heated combustion in material The easy decomposition combustion of organic group during burning, and discharge substantial amounts of heat.This will cause the calorific value of silica aerogel material Than larger, it has also become a great problem of restriction aerosil application.Therefore, a kind of dioxy of novel low value is developed SiClx aerogel material is extremely necessary.
The content of the invention
The technical problem that basic background technology is present, the present invention proposes a kind of low heat value aerosil composite wood Material and preparation method thereof, good flame resistance of the present invention, combustion heat value is low, while low combustion heat value is kept, moreover it is possible to avoid heat conduction The very big problem that coefficient and tap density become, makes thermal conductivity factor of the invention and tap density increase smaller, is maintained at relatively low Level.
The present invention proposes a kind of low heat value silicon dioxide silica aerogel composite material, and its raw material includes by weight:Dioxy 50-90 parts of SiClx aeroge, halogen-free flame retardants 5-40 parts, 1-10 parts of inorganic nano fire retarding synergist, opacifier 0.1-2 parts, point Powder 0.1-0.5 parts, lubricant 0.2-0.6 parts, reinforcing agent 1-5 parts.
Preferably, halogen-free flame retardants is phosphor nitrogen combustion inhibitor.
Preferably, halogen-free flame retardants is APP, ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium pyrophosphate, three The mixture of one or more compositions in poly cyanamid or melamine cyanurate.
Preferably, inorganic nano fire retarding synergist be nano-sized magnesium hydroxide, nano-aluminum hydroxide, nanometer double-hydroxide, The mixture of one or more compositions in nano titanium oxide, nano imvite or nanmeter antimong trioxide.
Preferably, opacifier is the mixed of one or more compositions in carbon black, carborundum, titanium dioxide, zirconium oxide Compound.
Preferably, dispersant is sodium tripolyphosphate, calgon, sodium pyrophosphate, triethyl group hexyl phosphoric acid, dodecyl Sodium sulphate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester or low molecular weight polycaprolactone second two One kind in alcohol.
Preferably, lubricant is talcum powder, magnesium stearate, cadmium stearate, copper stearate, barium stearate, zinc stearate, hard Resin acid calcium, stearmide, trihydroxy tristerin, lead stearate or stearic acid are polymerized with the low molecule of polyalcohol binary acid The mixture of one or more compositions in thing.
Preferably, reinforcing agent is glass fibre, boron fibre, alumina fibre, silicon carbide fibre, alloy fiber, metal fibre One kind in dimension, mullite fiber, brucite fiber, macromolecular fibre, zirconia fiber, ceramic fibre or epoxy resin or The mixture of two or more compositions.
The invention allows for the preparation method of above-mentioned low heat value silicon dioxide silica aerogel composite material, including following step Suddenly:Each raw material is uniformly mixed so as to obtain material A;By in abrading-ball and material A addition ball grinder, dispersion solvent is added, with 100- after sealing The speed of 300r/min, ball milling 6-10h takes out abrading-ball, is warming up to 60-120 DEG C, is dried to obtain low heat value aerosil Composite.
Preferably, abrading-ball is the one kind in agate abrading-ball, ceramic grinding ball, stainless steel abrading-ball.
Preferably, abrading-ball is made up of the bead that particle diameter is respectively 8mm, 11mm, 14mm, 20mm.
Preferably, abrading-ball and the volume ratio of material A are 2-3:1, and the addition of material A is not more than the three of ball milling tank volume / mono-.
Preferably, dispersion solvent is volatile polar solvent.
Preferably, dispersion solvent is in ethanol, methyl alcohol, acetone, tetrahydrofuran, isopropanol, n-butanol, n-hexane Kind.
Preferably, the tap density of low heat value silicon dioxide silica aerogel composite material is 0.08-0.5g/mL, thermal conductivity factor It is 0.022-0.0511W/ (mK).
The present invention is from aerosil and halogen-free flame retardants, inorganic nano fire retarding synergist, opacifier, dispersion Agent, lubricant, reinforcing agent are cooperated with proper ratio, while aerosil anti-flammability is increased, reduce dioxy The combustion heat value of SiClx aeroge;By the physical forces such as the friction in mechanical milling process, impact, extruding and friction process In Electrostatic Absorption so that halogen-free flame retardants, inorganic nano fire retarding synergist and aerosil mutually penetrate into and spread, Cooperated with dispersant, lubricant, it is dispersed, and opacifier, reinforcing agent and halogen-free flame retardants, inorganic nano can be promoted Fire retarding synergist, the counterdiffusion of aerosil phase, infiltration, absorption, form bridging, further form internal structure homogeneous Silica aerogel composite material, so as to increase anti-flammability of the invention, reduces combustion heat value of the invention;Halogen-free flameproof Agent and inorganic nano fire retarding synergist have flame retarding efficiency high, environmental protection, free from environmental pollution, the advantages of small toxicity, can be further Increase anti-flammability of the invention, and environmental protection;And the present invention is few using equipment, with short production cycle, flexible and convenient operation, equipment Operating cost is low;Each material cooperates while low combustion heat value is kept, moreover it is possible to avoid thermal conductivity factor and tap density from becoming Very big problem, make thermal conductivity factor of the invention and tap density increase smaller, be kept low.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of low heat value silicon dioxide silica aerogel composite material, its raw material includes by weight:Aerosil 70 Part, 20 parts of halogen-free flame retardants, 5 parts of inorganic nano fire retarding synergist, 1 part of opacifier, 0.3 part of dispersant, 0.4 part of lubricant increases Strong 3 parts of agent.
The preparation method of above-mentioned low heat value silicon dioxide silica aerogel composite material, comprises the following steps:Each raw material is mixed Obtain material A;By in abrading-ball and material A addition ball grinder, volatile polar solvent is added, with the speed of 200r/min after sealing Degree, ball milling 8h takes out abrading-ball, is warming up to 90 DEG C, is dried to obtain low heat value silicon dioxide silica aerogel composite material.
Embodiment 2
The raw material specified according to table 1 below, weighs each raw material by weight, and each raw material is uniformly mixed so as to obtain into material A;By agate Abrading-ball and material A are added in ball grinder, add ethanol, and with the speed of 100r/min after sealing, ball milling 10h takes out abrading-ball, heats up To 60 DEG C, be dried to obtain low heat value silicon dioxide silica aerogel composite material, wherein, agate abrading-ball by particle diameter be respectively 8mm, The bead composition of 11mm, 14mm, 20mm, abrading-ball is 2 with the volume ratio of material A:1.Then low heat value silica airsetting is detected The combustion heat value of glue composite, tap density, thermal conductivity factor, and compare with aerosil pure sample.
Table 1
Embodiment 3
The raw material specified according to table 2 below, weighs each raw material by weight, and each raw material is uniformly mixed so as to obtain into material A;By ceramics Abrading-ball and material A are added in ball grinder, add acetone, and with the speed of 300r/min after sealing, ball milling 6h takes out abrading-ball, heats up To 120 DEG C, be dried to obtain low heat value silicon dioxide silica aerogel composite material, wherein, ceramic grinding ball by particle diameter be respectively 8mm, The bead composition of 11mm, 14mm, 20mm, abrading-ball is 3 with the volume ratio of material A:1.Then low heat value silica airsetting is detected The combustion heat value of glue composite, tap density, thermal conductivity factor, and compare with aerosil pure sample.
Table 2
Embodiment 4
The raw material specified according to table 3 below, weighs each raw material by weight, and each raw material is uniformly mixed so as to obtain into material A;Will be stainless Steel abrading-ball and material A are added in ball grinder, add n-hexane, and with the speed of 200r/min after sealing, ball milling 8h takes out abrading-ball, 80 DEG C are warming up to, low heat value silicon dioxide silica aerogel composite material is dried to obtain, wherein, stainless steel abrading-ball is respectively by particle diameter The bead composition of 8mm, 11mm, 14mm, 20mm, abrading-ball is 2.5 with the volume ratio of material A:1.Then low heat value titanium dioxide is detected The combustion heat value of silica aerogel composite, tap density, thermal conductivity factor, and compare with aerosil pure sample.
Table 3
Embodiment 5
The raw material specified according to table 4 below, weighs each raw material by weight, and each raw material is uniformly mixed so as to obtain into material A;By agate Abrading-ball and material A are added in ball grinder, are taken out abrading-ball, are heated up with the speed of 200r/min, ball milling 8h after adding isopropanol sealing To 100 DEG C, be dried to obtain low heat value silicon dioxide silica aerogel composite material, wherein, agate abrading-ball by particle diameter be respectively 8mm, The bead composition of 11mm, 14mm, 20mm, abrading-ball is 3 with the volume ratio of material A:1.Then low heat value silica airsetting is detected The combustion heat value of glue composite, tap density, thermal conductivity factor, and compare with aerosil pure sample.
Table 4
By embodiment 2-5, it can be seen that combustion heat value of the invention is low, and thermal conductivity factor of the invention and tap density with Aerosil pure sample is smaller compared to increasing, and is kept low.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.

Claims (10)

1. a kind of low heat value silicon dioxide silica aerogel composite material, it is characterised in that its raw material includes by weight:Silica Aeroge 50-90 parts, halogen-free flame retardants 5-40 parts, 1-10 parts of inorganic nano fire retarding synergist, opacifier 0.1-2 parts, dispersant 0.1-0.5 parts, lubricant 0.2-0.6 parts, reinforcing agent 1-5 parts.
2. low heat value silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that halogen-free flame retardants is phosphorus Nitrogen combustion inhibitor.
3. low heat value silicon dioxide silica aerogel composite material according to claim 1, it is characterised in that halogen-free flame retardants is poly- One kind in ammonium phosphate, ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium pyrophosphate, melamine or melamine cyanurate Or the mixture of two or more compositions.
4. the low heat value silicon dioxide silica aerogel composite material according to claim any one of 1-3, it is characterised in that inorganic to receive Rice fire retarding synergist is nano-sized magnesium hydroxide, nano-aluminum hydroxide, nanometer double-hydroxide, nano titanium oxide, nanometer cover de- The mixture of one or more compositions in soil or nanmeter antimong trioxide.
5. the low heat value silicon dioxide silica aerogel composite material according to claim any one of 1-4, it is characterised in that opacifier It is the mixture of one or more compositions in carbon black, carborundum, titanium dioxide, zirconium oxide.
6. the low heat value silicon dioxide silica aerogel composite material according to claim any one of 1-5, it is characterised in that dispersant It is sodium tripolyphosphate, calgon, sodium pyrophosphate, triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, fiber One kind in plain derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester or low-molecular-weight polyethylene glycol.
7. the low heat value silicon dioxide silica aerogel composite material according to claim any one of 1-6, it is characterised in that lubricant It is talcum powder, magnesium stearate, cadmium stearate, copper stearate, barium stearate, zinc stearate, calcium stearate, stearmide, three hydroxyls One or more in the low polymer of base tristerin, lead stearate or stearic acid and polyalcohol binary acid The mixture of composition.
8. the low heat value silicon dioxide silica aerogel composite material according to claim any one of 1-7, it is characterised in that reinforcing agent For glass fibre, boron fibre, alumina fibre, silicon carbide fibre, alloy fiber, metallic fiber, mullite fiber, shepardite are fine The mixture of one or more compositions in dimension, macromolecular fibre, zirconia fiber, ceramic fibre or epoxy resin.
9. a kind of preparation method of the low heat value silicon dioxide silica aerogel composite material as described in claim any one of 1-8, it is special Levy and be, comprise the following steps:Each raw material is uniformly mixed so as to obtain material A;By in abrading-ball and material A addition ball grinder, dispersion is added Solvent, with the speed of 100-300r/min after sealing, ball milling 6-10h takes out abrading-ball, is warming up to 60-120 DEG C, is dried to obtain low Calorific value silicon dioxide silica aerogel composite material.
10. according to the preparation method of low heat value silicon dioxide silica aerogel composite material as claimed in claim 9, it is characterised in that Abrading-ball is the one kind in agate abrading-ball, ceramic grinding ball, stainless steel abrading-ball;Preferably, abrading-ball by particle diameter be respectively 8mm, 11mm, The bead composition of 14mm, 20mm;Preferably, abrading-ball and the volume ratio of material A are 2-3:1, and the addition of material A is not more than ball / 3rd of grinding jar volume;Preferably, dispersion solvent is volatile polar solvent;Preferably, dispersion solvent is ethanol, first One kind in alcohol, acetone, tetrahydrofuran, isopropanol, n-butanol, n-hexane;Preferably, low heat value aerosil is combined The tap density of material is 0.08-0.5g/mL, and thermal conductivity factor is 0.022-0.0511W/ (mK).
CN201611132215.4A 2016-12-09 2016-12-09 A kind of low heat value silicon dioxide silica aerogel composite material and preparation method thereof Pending CN106753437A (en)

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Cited By (5)

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CN108483974A (en) * 2018-04-01 2018-09-04 中鸿纳米纤维技术丹阳有限公司 A kind of simplex method prepares silica aerogel composite reinforcing material
CN109081354A (en) * 2017-06-14 2018-12-25 天津城建大学 Fire-retardant galapectite-silicon dioxide composite aerogel material and preparation method thereof
CN109851380A (en) * 2019-03-01 2019-06-07 谢吉萍 A kind of preparation method of aerosil functional material
CN112679789A (en) * 2021-01-20 2021-04-20 江苏威久科技发展有限公司 Flame-retardant n-pentane foaming agent for polyurethane and preparation method thereof
CN117510181A (en) * 2023-11-07 2024-02-06 武汉中科先进材料科技有限公司 Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof

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CN109081354A (en) * 2017-06-14 2018-12-25 天津城建大学 Fire-retardant galapectite-silicon dioxide composite aerogel material and preparation method thereof
CN108483974A (en) * 2018-04-01 2018-09-04 中鸿纳米纤维技术丹阳有限公司 A kind of simplex method prepares silica aerogel composite reinforcing material
CN109851380A (en) * 2019-03-01 2019-06-07 谢吉萍 A kind of preparation method of aerosil functional material
CN112679789A (en) * 2021-01-20 2021-04-20 江苏威久科技发展有限公司 Flame-retardant n-pentane foaming agent for polyurethane and preparation method thereof
CN117510181A (en) * 2023-11-07 2024-02-06 武汉中科先进材料科技有限公司 Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof
CN117510181B (en) * 2023-11-07 2024-04-16 武汉中科先进材料科技有限公司 Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof

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Application publication date: 20170531