CN104556964A - Hydrophobic silica aerogel heat-insulation composite material and preparation method thereof - Google Patents
Hydrophobic silica aerogel heat-insulation composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hydrophobic silica aerogel heat-insulation composite material and a preparation method thereof. The composite material consists of silica aerogel and an inorganic fiber product, wherein the silica aerogel is doped with a flame retardant and an infrared blocking agent. During preparation of sol, siloxane containing hydrophobic groups is introduced, and the content and the distribution state of the hydrophobic groups in a system are controlled by controlling the reactant content and reaction conditions, so that the composite material can pass the test of GB8624-2012 Classification for Burning Behavior of Building Materials and Products (A1-level). The preparation method of the composite material comprises steps as follows: (1) preparation of the silica sol; (2) preparation of composite gel; (3) solvent replacement; (4) drying. With the adoption of the method, the process is simple, the production cycle is short, the cost is lower, the equipment requirement is low, and the prepared silica aerogel composite material has the overall waterproof performance, the extremely low heat conductivity coefficient and the excellent high-temperature heat-insulation performance.
Description
Technical field
The present invention relates to a kind of aerogel insulating material and preparation method thereof, particularly relate to a kind of hydrophobic type aerosil heat insulation composite material and preparation method thereof.
Background technology
Aerosil is the nano-meter porous amorphous state solid material of a kind of low density, high porosity, transmittance is higher, also referred to as " blue smoke ", " solid cigarette ", gaseous state dispersion medium is full of in hole, there is continuous print nanoscale three-dimensional network structure and hole, be at present known in the world density minimum and the minimum solid material of thermal conductivity.Its bore hole size and network skeleton are nano level, bore hole size distribution range is 1 ~ 100 nanometer, network skeleton particle size distribution range is 1 ~ 30 nanometer, this special construction makes it have high porosity (80% ~ 99.8%), low density (3 ~ 250kg/m3), high-specific surface area (500 ~ 1000m2/g), low-k (1.1 ~ 2.5), low thermal conductivity (0.013 ~ 0.025w/(mk)) etc. feature, at mechanics, acoustics, calorifics, the many-sides such as optics have peculiar property, in space flight and aviation, military project, petrochemical industry, mineral products, electronics, medical, metallurgy etc. field has broad application prospects.
The modal technique of hydrophobic type aerosil is silylanizing surface modification.Greatly mainly with tetraethoxy, methyl silicate, water glass etc. for silicon source is hydrolyzed polycondensation, after forming gel, silylanizing modification is carried out to gel, carry out supercritical drying, subcritical drying or constant pressure and dry again, the aerogel prepared has preferably hydrophobic performance and heat-proof quality, can be applicable to more field.
Patent CN1126591C, CN1087172C, CN1126591C take water glass as silicon source, under acidic ion exchange resin, mineral acid or hydrochloric acid solution's effect, regulate sodium silicate solution to pH≤3, then carry out the silicic acid of polycondensation gained by adding alkali, form silica dioxide gel; After again silica dioxide gel sillylation reagent being carried out surface modification, obtain hydrophobic aerosil through subcritical drying.
Patent CN101503195A take tetraethoxy as silicon source, being mixed in container to seal with dehydrated alcohol, oxalic acid solution is placed in water-bath, add ammoniacal liquor after hydrolysis and form gel, with the water in dehydrated alcohol displacement gel, with the ethanol in normal hexane displacement gel, with the mixed solution of properties-correcting agent and normal hexane, surface modification is carried out to gel again, then replace unreacted properties-correcting agent with normal hexane, finally put into baking oven classification drying and obtain aerogel.The aerogel obtained by power method has the advantages such as porosity is high, specific surface area is large, hydrophobicity is good.
When preparing silica dioxide gel with traditional silicon source, its forming process is Si(OH)
4the process of continuous crosslinking polymerization, this just determines silica dioxide gel surface and there is many-OH that cannot be cross-linked, and the modifying process of silica dioxide gel is exactly the process that-OH is replaced by hydrophobic grouping, in modifying process, surface-modifying agent spreads gradually from the outside past inside of gel and reacts, so only the complete modification guarantee material monolithic of guaranteed gel surface-OH is hydrophobic with-OH.So containing a large amount of hydrophobic groupings in the hydrophobic aerogels prepared of traditional technology or aerogel composite, and the surface-modifying agent of a large amount of ADSORPTION STATE, usually more than 250 DEG C, surface-modifying agent is desorption gradually, and evaporate in the form of a vapor, run into oxygen and high temperature can be oxidized; When temperature is more than 450 DEG C, hydrophobic grouping also will be broken down and oxidized.Therefore, when the environment of more than 500 DEG C put into by the aerosil that traditional technology is prepared from and matrix material thereof, inevitably there will be high temperature exothermic and catching fire phenomenon, be difficult to by the detection of GB8624-2012 material of construction and product burns grading performance (A1 level) thereof (testing requirement under the high temperature of 750 DEG C without burning, or flame duration is no more than 20s), thus make aerogel products use under some high request condition and there is potential safety hazard, also limit range of application and the market of aerogel products.Use the use of surface-modifying agent also can bring HUMAN HEALTH and production safety in traditional technology in a large number to a certain degree to affect simultaneously.
Summary of the invention
For the above-mentioned technical problem of prior art, the object of this invention is to provide a kind of hydrophobic type aerosil heat insulation composite material and preparation method thereof, present invention process is simple, with short production cycle, cost is lower, equipment requirements is low, reaction conditions is controlled, excellent product performance, the silicon dioxide silica aerogel composite material of preparation has integral waterproofing performance, extremely low thermal conductivity, excellent high-temperature heat insulation performance, detect by uninflammability when ensureing that material monolithic is hydrophobic, its uninflammability detects and reaches A1 level.
For achieving the above object, the present invention is achieved by the following technical solutions:
A kind of hydrophobic type aerosil heat insulation composite material, be made up of aerosil and inorganic fibre goods, described aerosil is doped with fire retardant and infrared barrier agent; Described inorganic fibre goods are one or more in glass fibre, quartz glass fibre, aluminum silicate fiber, ceramic fiber, sapphire whisker, Zirconium oxide fibre, rock wool fibers, basalt fibre, and the porosity of inorganic fibre goods is more than 50%, be preferably more than 60%, be more preferably more than 70%.
Described fire retardant is one or both mixtures of inorganic combustion inhibitor or organic halogen-free environment-friendlyflame flame retardant; Described inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant used in combination, the mass ratio of inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant is 0.1 ~ 100:1, be preferably 0.1 ~ 80:1.
Described inorganic combustion inhibitor is one or more of magnesium hydroxide, aluminium hydroxide, zinc borate, ammonium polyphosphate, red phosphorus, weisspiessglanz or molybdenum compound; Described organic halogen-free environment-friendlyflame flame retardant is poly phosphate, trimeric cyanamide, three (1-oxo-1-phosphas-2,6,7-trioxa-l-phosphabicyclo [2,2,2] octane-4-methylene radical) one or more of phosphoric acid ester, N, N-Ursol D base (2-hydroxyl) dibenzyl phosphonic acids tetra-ethyl ester, melamine phosphate or melamine cyanurate.
Described infrared barrier agent is one or more mixtures of the agent of absorbing radiation type infrared barrier, the agent of conductor oxidate infrared barrier or the agent of reflection-type infrared barrier; Described absorbing radiation type infrared barrier agent is metal oxide, the agent of absorbing radiation type infrared barrier can also be Multimetal oxide through the mixture of high temperature dopant or carbide, and described metal oxide is ferric oxide, manganese oxide, cupric oxide, nickel oxide, chromic oxide, lanthanum trioxide, cobalt oxide or one or more mixtures zirconic; Described conductor oxidate infrared barrier agent is one or more mixtures of tin indium oxide, tin-antiomony oxide or aluminum zinc oxide; Described reflection-type infrared barrier agent is one or more mixtures of mica powder, talcum powder, trichroite, titanium oxide or zinc oxide.
A preparation method for hydrophobic type aerosil heat insulation composite material, comprises the following steps:
(1) preparation of silicon dioxide gel: take siloxanes as presoma, by multiple siloxanes mixing and stirring, add organic solvent, water again, stir, maintain and stir, more dropwise add an acidic catalyst regulator solution pH value to 1 ~ 6, be preferably 1 ~ 5,0 DEG C ~ 70 DEG C constant temperature more than 6 hours, be preferably 30 ~ 70 DEG C of constant temperature more than 8 hours, obtain the silicon dioxide gel clarified; The mol ratio of described siloxanes, organic solvent, water is 1:1 ~ 80:2 ~ 40, is preferably 1:1 ~ 70:2 ~ 30.By the optimization of the mol ratio to siloxanes, organic solvent, water, the porosity of aerogel, specific surface area, density and organic content can be regulated, obtain the aerosil that performance is better.
By the optimization to silicon dioxide gel preparation condition, the sol particle particle diameter that obtains can be made evenly, organic group is more evenly distributed, make the intensity of the aerogel composite of preparation and hydrophobicity more excellent.
(2) preparation of plural gel: fire retardant, infrared barrier agent are joined in the silicon dioxide gel of step (1) in the ratio of every 1L silicon dioxide gel doping 1g ~ 100g fire retardant, the agent of 1g ~ 100g infrared barrier, rapid dispersed with stirring is even, obtains the silicon dioxide gel adulterated; Dropwise add basic catalyst adjust ph to 6 ~ 7 again.
Inorganic fibre goods are immersed in above-mentioned silicon dioxide gel, leave standstill 0.01 ~ 72 hour at 0 DEG C ~ 80 DEG C; Obtain plural gel, at 0 DEG C ~ 80 DEG C aging 0 ~ 96 hour.
(3) solvent exchange: the plural gel after aging in use organic solvent displacement step (2), displacement temperature is 0 ~ 80 DEG C, 1 ~ 48 hour time, number of times 1 ~ 10 time.
(4) dry: the plural gel of step (3) gained to be carried out drying and obtains hydrophobic type aerosil heat insulation composite material.
Siloxanes in described step (1) is Si(OR
1)
4with R
2si(OR
3)
3, R
4 2si(OR
5)
2, R
6 3si(OR
7) in the mixture of one or more, described R
1, R
2, R
3, R
4, R
5, R
6and R
7can be identical or different alkane, alkene, aromatic hydrocarbon group.Preferred Si(OR
1)
4with R
2si(OR
3)
3, R
3 2si(OR
4)
2in one or both mixture.Si(OR
1)
4be 1:0.1 ~ 15 with the mol ratio of siloxanes containing hydrophobic grouping, preferred 1:0.2 ~ 10.By the optimization to each component molar ratio in siloxane precursors mixing, the structure of aerosil can be improved, strengthen its mechanical property, control the content of the organic group in aerogel.
An acidic catalyst in described step (1) is mineral acid or organic acid; Described mineral acid is HCl, H
2sO
4, H
3pO
4, H
2cO
3, HF, HBr, HNO
3, H
2sO
3or HClO
4one or more mixtures, described organic acid is CH
3cOOH, HOOC-COOH, HOOCC
2h
4cOOH or C
6h
5one or more mixtures of COOH.
Organic solvent in described step (1) is one or more in methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol or acetone; Organic solvent in described step (3) is one or more of methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol, acetone, butanone, normal hexane, isohexane, heptane or octane.
Leaving standstill in described step (2) is 20 ~ 80 DEG C, 0.01 ~ 36 hour; Aging is 30 ~ 80 DEG C, 0 ~ 48 hour.
Be replaced into 30 ~ 80 DEG C in described step (3), the time is 1 ~ 36 hour, and number of times is 1 ~ 4 time.
The method of the drying in described step (4) is one or more in supercritical drying, constant pressure and dry, subcritical drying, vacuum-drying or lyophilize; The medium of described supercritical drying, subcritical drying is the one in carbonic acid gas, methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols, acetone or acetonitrile; Described constant pressure and dry temperature is 20 ~ 200 DEG C, and the time is 0.1 ~ 160h, and preferred drying temperature is 40 ~ 200 DEG C, and preferred time of drying is 0.5 ~ 120h.
The preparation method of hydrophobic type aerosil heat insulation composite material of the present invention, drive in body process before the reaction, introduce the siloxanes containing hydrophobic grouping, and by the hydrophobic group content in control reactant content and reaction conditions and then the hierarchy of control and distribution, thus the gel surface modified technique in cancellation traditional technology, avoid the hydrophobizing agent of ADSORPTION STATE, and ensureing, under overall hydrophobic condition, significantly to reduce surface hydrophobicity group; Be doped into fire retardant in the collosol and gel stage, significantly promote the flame retardant properties of silicon dioxide silica aerogel composite material; Infrared barrier agent is doped in the collosol and gel stage, significantly promote the high temperature insulating performance of silicon dioxide silica aerogel composite material, make that the hydrophobic type aerosil heat insulation composite material obtained has hydrophobic surface group, entirety is hydrophobic, hydrophobic performance is excellent, and can be detected by " GB8624-2012 material of construction and product burns grading performance (A1 level) thereof ".
The present invention has following beneficial effect compared with traditional technology:
1, production technique of the present invention is simple, easy to operate.The present invention abandons using traditional single organic or inorganic silicon source, then adopts the multiple siloxanes containing hydrophobic grouping to mix as presoma, introduces hydrophobic grouping, can save traditional surface modification step when prepared by silicon dioxide gel.Hydrophobic grouping simultaneously owing to introducing in advance, effectively can reduce time swap during solvent exchange, and a large amount of number of times reducing solvent exchange.
2, controllability of the present invention is good.The present invention adopts the multiple siloxanes containing hydrophobic grouping to mix as presoma, compare with traditional technology, make hydrophobic grouping being more evenly distributed in system inside, nucleation process and the polymerization process of sol particle are more stable, the network structure of gel is more complete, even, make that aerosil density is better, specific surface area is larger, porosity is higher and void distribution is better, obtains the silicon dioxide silica aerogel composite material of excellent performance.
3, the present invention is by the mol ratio of siloxanes, alcoholic solvent, water in mole when reaction system that regulates each component in siloxanes, the hydrophobic group content in reaction system is greatly reduced while ensureing hydrophobic performance, novelty be doped into fire retardant in the collosol and gel stage, be doped with the infrared barrier agent of infrared barrier excellent performance simultaneously, significantly promote the heat-proof quality of this matrix material when high temperature.This hydrophobic type aerosil felt insulation can be detected by GB8624-2012 material of construction and product burns grading performance (A1 level) thereof.
4, cost of the present invention is low, security is high.The present invention introduces hydrophobic grouping when prepared by silicon dioxide gel, eliminates traditional surface modification step, namely eliminates the expense of a large amount of surface modification agent, and avoids in preparation process the potential safety hazard using exhibiting high surface modified solution to bring.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
The raw material adopted in the present invention all can obtain by means commonly known in the art, also can adopt commercially available prod.
The preparation method of hydrophobic type aerosil heat insulation composite material of the present invention, comprises the following steps:
(1) preparation of silicon dioxide gel: take siloxanes as presoma, by multiple siloxanes mixing and stirring, add organic solvent, water again, stir, maintain and stir, more dropwise add an acidic catalyst regulator solution pH value to 1 ~ 6, be preferably 1 ~ 5,0 DEG C ~ 70 DEG C constant temperature more than 6 hours, be preferably 30 ~ 70 DEG C of constant temperature more than 8 hours, obtain the silicon dioxide gel clarified; The mol ratio of described siloxanes, organic solvent, water is 1:1 ~ 80:2 ~ 40, is preferably 1:1 ~ 70:2 ~ 30.By the optimization of the mol ratio to siloxanes, organic solvent, water, the porosity of aerogel, specific surface area, density and organic content can be regulated, obtain the aerosil that performance is better.
Siloxanes is Si(OR
1)
4with R
2si(OR
3)
3, R
4 2si(OR
5)
2, R
6 3si(OR
7) in the mixture of one or more, described R
1, R
2, R
3, R
4, R
5, R
6and R
7can be identical or different alkane, alkene, aromatic hydrocarbon group.Preferred Si(OR
1)
4with R
2si(OR
3)
3, R
3 2si(OR
4)
2in one or both mixture.Si(OR
1)
4be 1:0.1 ~ 15 with the mol ratio of siloxanes containing hydrophobic grouping, preferred 1:0.2 ~ 10.By the optimization to each component molar ratio in siloxane precursors mixing, the structure of aerosil can be improved, strengthen its mechanical property, control the content of the organic group in aerogel.
Organic solvent is one or more in methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol or acetone.
An acidic catalyst is mineral acid or organic acid; Described mineral acid is HCl, H
2sO
4, H
3pO
4, H
2cO
3, HF, HBr, HNO
3, H
2sO
3or HClO
4one or more mixtures, described organic acid is CH
3cOOH, HOOC-COOH, HOOCC
2h
4cOOH or C
6h
5one or more mixtures of COOH.
By the optimization to silicon dioxide gel preparation condition, the sol particle particle diameter that obtains can be made evenly, organic group is more evenly distributed, make the intensity of the aerogel composite of preparation and hydrophobicity more excellent.
(2) preparation of plural gel: fire retardant, infrared barrier agent are joined in the silicon dioxide gel of step (1) in the ratio of every 1L silicon dioxide gel doping 1g ~ 100g fire retardant, the agent of 1g ~ 100g infrared barrier, rapid dispersed with stirring is even, obtains the silicon dioxide gel adulterated; Dropwise add basic catalyst adjust ph to 6 ~ 7 again.
Inorganic fibre goods are immersed in above-mentioned silicon dioxide gel, leave standstill 0.01 ~ 72 hour at 0 DEG C ~ 80 DEG C, be preferably 20 ~ 80 DEG C, 0.01 ~ 36 hour; Obtain plural gel, at 0 DEG C ~ 80 DEG C aging 0 ~ 96 hour, be preferably 30 ~ 80 DEG C, 0 ~ 48 hour.
(3) solvent exchange: the plural gel after aging in use organic solvent displacement step (2), displacement temperature is 0 ~ 80 DEG C, 1 ~ 48 hour time, number of times 1 ~ 10 time; Preferred displacement temperature is 30 ~ 80 DEG C, and the time is 1 ~ 36 hour, and number of times is 1 ~ 4 time.Organic solvent is one or more of methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol, acetone, butanone, normal hexane, isohexane, heptane or octane.
(4) dry: the plural gel of step (3) gained to be carried out drying and obtains hydrophobic type aerosil heat insulation composite material.Dry method is one or more in supercritical drying, constant pressure and dry, subcritical drying, vacuum-drying or lyophilize; The medium of described supercritical drying, subcritical drying is the one in carbonic acid gas, methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols, acetone or acetonitrile; Described constant pressure and dry temperature is 20 ~ 200 DEG C, and the time is 0.1 ~ 160h, and preferred drying temperature is 40 ~ 200 DEG C, and preferred time of drying is 0.5 ~ 120h.
The hydrophobic type aerosil heat insulation composite material that the present invention obtains, is made up of aerosil and inorganic fibre goods, and aerosil is doped with fire retardant and infrared barrier agent; Inorganic fibre goods are one or more in glass fibre, quartz glass fibre, aluminum silicate fiber, ceramic fiber, sapphire whisker, Zirconium oxide fibre, rock wool fibers, basalt fibre, and the porosity of inorganic fibre goods is more than 50%, be preferably more than 60%, be more preferably more than 70%.
Fire retardant is one or both mixtures of inorganic combustion inhibitor or organic halogen-free environment-friendlyflame flame retardant; Described inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant used in combination, the mass ratio of inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant is 0.1 ~ 100:1, be preferably 0.1 ~ 80:1.
Inorganic combustion inhibitor be magnesium hydroxide, aluminium hydroxide, zinc borate, ammonium polyphosphate, red phosphorus, weisspiessglanz, molybdenum compound one or more; Described organic halogen-free environment-friendlyflame flame retardant is poly phosphate, trimeric cyanamide, three (1-oxo-1-phosphas-2,6,7-trioxa-l-phosphabicyclo [2,2,2] octane-4-methylene radical) phosphoric acid ester, N, N-Ursol D base (2-hydroxyl) dibenzyl phosphonic acids tetra-ethyl ester, melamine phosphate, melamine cyanurate one or more.
Infrared barrier agent is one or more mixtures of the agent of absorbing radiation type infrared barrier, the agent of conductor oxidate infrared barrier or the agent of reflection-type infrared barrier; Described absorbing radiation type infrared barrier agent is metal oxide, the agent of absorbing radiation type infrared barrier can also be Multimetal oxide through the mixture of high temperature dopant or carbide, and described metal oxide is ferric oxide, manganese oxide, cupric oxide, nickel oxide, chromic oxide, lanthanum trioxide, cobalt oxide, one or more mixtures zirconic; Described conductor oxidate infrared barrier agent is one or more mixtures of tin indium oxide, tin-antiomony oxide, aluminum zinc oxide; Described reflection-type infrared barrier agent is one or more mixtures of mica powder, talcum powder, trichroite, titanium oxide, zinc oxide.
embodiment 1
By methyl silicate, vinyltrimethoxy silane with the ratio mixing and stirring of mol ratio 1:8, then by this mixture and propyl alcohol, water with the abundant mixing and stirring of the ratio of mol ratio 1:40:3, with the H of 3mol/L
2sO
4solution slowly instills in the solution mixed, and limit is stirred to become and dripped, regulator solution pH value to 1, then the solution Keep agitation 10 hours obtained silicon dioxide gels at 50 DEG C that will prepare.In the ratio of every 1L silicon dioxide gel doping 5g zinc borate, 5g ammonium polyphosphate, 5g nickel oxide, fire retardant, infrared barrier agent are doped in colloidal sol, abundant mixing and stirring, then use ammonia soln adjust ph to 6.Ceramic fiber blanket is immersed the silicon dioxide gel of doping, be placed in 40 DEG C of water-baths, after 30 hours, form silicon-dioxide plural gel.Continue in 60 DEG C of water-baths aging 20 hours.Taken out by plural gel, replace with propyl alcohol, the ratio of propyl alcohol and gel is 5:1, displacement temperature is 40 DEG C, and time swap is 30 hours, altogether replaces 2 times, obtain compound alcogel, then through ethanol supercritical drying, namely obtain hydrophobic type silicon dioxide composite material.Obtained hydrophobic type silicon dioxide composite material hydrophobicity is good, thermal conductivity 0.0185w/(mk).Can be detected by " GB8624-2012 material of construction and product burns grading performance (A1 level) thereof ".
embodiment 2
By tetraethoxy, diethyldiethoxysilane with the ratio mixing and stirring of mol ratio 1:6, again by this mixture, dehydrated alcohol, water with the abundant mixing and stirring of the ratio of mol ratio 1:50:8, slowly instill in the solution mixed with the HOOC-COOH solution of 2mol/L, limit is stirred to become and is dripped, regulator solution pH value to 5, then the solution Keep agitation 12 hours obtained silicon dioxide gels at 50 DEG C that will prepare.In the ratio of every 1L silicon dioxide gel doping 3g weisspiessglanz, 6g melamine phosphate, 3g tin indium oxide, fire retardant, infrared barrier agent are doped in colloidal sol, abundant mixing and stirring, then use ammonia soln adjust ph to 6.3.Basalt fibre felt is immersed the silicon dioxide gel of doping, be placed in 60 DEG C of water-baths, after 8 hours, form silicon-dioxide plural gel.Continue in 50 DEG C of water-baths aging 24 hours.Taken out by plural gel, replace with dehydrated alcohol, the ratio of dehydrated alcohol and gel is 5:1, and displacement temperature is 50 DEG C, and time swap is 24h, altogether replaces 3 times, obtains compound alcogel; The compound alcogel normal hexane obtained is replaced, and the ratio of normal hexane and gel is 5:1, and displacement temperature is 60 DEG C, and time swap is 8h, altogether replaces 4 times, then through constant pressure and dry, 60 DEG C 72 hours, namely obtain hydrophobic type silicon dioxide composite material.Obtained hydrophobic type silicon dioxide composite material hydrophobicity is good, thermal conductivity 0.022w/(mk).Can be detected by " GB8624-2012 material of construction and product burns grading performance (A1 level) thereof ".
embodiment 3
By tetraethoxy, vinyl triethoxyl, diethyldiethoxysilane with the ratio mixing and stirring of mol ratio 1:4:3, then by this mixture, acetone, water with the abundant mixing and stirring of the ratio of mol ratio 1:60:4, with the CH of 2mol/L
3cOOH solution slowly instills in the solution mixed, and limit is stirred to become and dripped, regulator solution pH value to 4, then the solution Keep agitation 24 hours obtained silicon dioxide gels at 40 DEG C that will prepare.By every 1L silicon dioxide gel doping 6g magnesium hydroxide, 2g N, fire retardant, infrared barrier agent are doped in colloidal sol by the ratio of N-Ursol D base (2-hydroxyl) dibenzyl phosphonic acids tetra-ethyl ester, 5g titanium oxide, abundant mixing and stirring, then use ammonia soln adjust ph to 6.5.Glass mat is immersed the silicon dioxide gel of doping, be placed in 50 DEG C of water-baths, after 16 hours, form silicon-dioxide plural gel.In 50 DEG C of water-baths aging 36 hours.Taken out by plural gel, replace with acetone, the ratio of acetone and gel is 5:1, displacement temperature is 50 DEG C, and time swap is 16h, altogether replaces 3 times, obtain compound alcogel, drier through CO 2 supercritical, namely obtain hydrophobic type silicon dioxide composite material.Obtained hydrophobic type silicon dioxide composite material hydrophobicity is good, thermal conductivity 0.021w/(mk).Can be detected by " GB8624-2012 material of construction and product burns grading performance (A1 level) thereof ".
The preparation method of hydrophobic type aerosil heat insulation composite material of the present invention, drive in body process before the reaction, introduce the siloxanes containing hydrophobic grouping, and by the hydrophobic group content in control reactant content and reaction conditions and then the hierarchy of control and distribution, thus the gel surface modified technique in cancellation traditional technology, avoid the hydrophobizing agent of ADSORPTION STATE, and ensureing, under overall hydrophobic condition, significantly to reduce surface hydrophobicity group; Be doped into fire retardant in the collosol and gel stage, significantly promote the flame retardant properties of silicon dioxide silica aerogel composite material; Infrared barrier agent is doped in the collosol and gel stage, significantly promote the high temperature insulating performance of silicon dioxide silica aerogel composite material, make that the hydrophobic type aerosil heat insulation composite material obtained has hydrophobic surface group, entirety is hydrophobic, hydrophobic performance is excellent, and can be detected by " GB8624-2012 material of construction and product burns grading performance (A1 level) thereof ".
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (10)
1. a hydrophobic type aerosil heat insulation composite material, is characterized in that: be made up of aerosil and inorganic fibre goods, and described aerosil is doped with fire retardant and infrared barrier agent; Described inorganic fibre goods are one or more in glass fibre, quartz glass fibre, aluminum silicate fiber, ceramic fiber, sapphire whisker, Zirconium oxide fibre, rock wool fibers or basalt fibre, and the porosity of inorganic fibre goods is more than 50%.
2. hydrophobic type aerosil heat insulation composite material as claimed in claim 1, is characterized in that: described fire retardant is one or both mixtures of inorganic combustion inhibitor or organic halogen-free environment-friendlyflame flame retardant; Described inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant used in combination, the mass ratio of inorganic combustion inhibitor and organic halogen-free environment-friendlyflame flame retardant is 0.1 ~ 100:1; Described inorganic combustion inhibitor is one or more of magnesium hydroxide, aluminium hydroxide, zinc borate, ammonium polyphosphate, red phosphorus, weisspiessglanz or molybdenum compound; Described organic halogen-free environment-friendlyflame flame retardant is poly phosphate, trimeric cyanamide, three (1-oxo-1-phosphas-2,6,7-trioxa-l-phosphabicyclo [2,2,2] octane-4-methylene radical) one or more of phosphoric acid ester, N, N-Ursol D base (2-hydroxyl) dibenzyl phosphonic acids tetra-ethyl ester, melamine phosphate or melamine cyanurate.
3. hydrophobic type aerosil heat insulation composite material as claimed in claim 1, is characterized in that: described infrared barrier agent is one or more mixtures of the agent of absorbing radiation type infrared barrier, the agent of conductor oxidate infrared barrier or the agent of reflection-type infrared barrier; Described absorbing radiation type infrared barrier agent is metal oxide, the agent of absorbing radiation type infrared barrier can also be Multimetal oxide through the mixture of high temperature dopant or carbide, and described metal oxide is ferric oxide, manganese oxide, cupric oxide, nickel oxide, chromic oxide, lanthanum trioxide, cobalt oxide or one or more mixtures zirconic; Described conductor oxidate infrared barrier agent is one or more mixtures of tin indium oxide, tin-antiomony oxide or aluminum zinc oxide; Described reflection-type infrared barrier agent is one or more mixtures of mica powder, talcum powder, trichroite, titanium oxide or zinc oxide.
4. a preparation method for the hydrophobic type aerosil heat insulation composite material as described in claim as arbitrary in claim 1-3, is characterized in that comprising the following steps:
(1) preparation of silicon dioxide gel: take siloxanes as presoma, by multiple siloxanes mixing and stirring, add organic solvent, water again, stir, maintain and stir, dropwise add an acidic catalyst regulator solution pH value to 1 ~ 6 again, 0 DEG C ~ 70 DEG C constant temperature more than 6 hours, obtain the silicon dioxide gel clarified; The mol ratio of described siloxanes, organic solvent, water is 1:1 ~ 80:2 ~ 40;
(2) preparation of plural gel: fire retardant, infrared barrier agent are joined in the silicon dioxide gel of step (1) in the ratio of every 1L silicon dioxide gel doping 1g ~ 100g fire retardant, the agent of 1g ~ 100g infrared barrier, rapid dispersed with stirring is even, obtains the silicon dioxide gel adulterated; Dropwise add basic catalyst adjust ph to 6 ~ 7 again;
Inorganic fibre goods are immersed in above-mentioned silicon dioxide gel, leave standstill 0.01 ~ 72 hour at 0 DEG C ~ 80 DEG C, obtain plural gel, at 0 DEG C ~ 80 DEG C aging 0 ~ 96 hour;
(3) solvent exchange: the plural gel after aging in use organic solvent displacement step (2), displacement temperature is 0 ~ 80 DEG C, 1 ~ 48 hour time, number of times 1 ~ 10 time;
(4) dry: the plural gel of step (3) gained to be carried out drying and obtains hydrophobic type aerosil heat insulation composite material.
5. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, is characterized in that: the siloxanes in described step (1) is Si(OR
1)
4with R
2si(OR
3)
3, R
4 2si(OR
5)
2, R
6 3si(OR
7) in the mixture of one or more, described R
1, R
2, R
3, R
4, R
5, R
6and R
7can be identical or different alkane, alkene, aromatic hydrocarbon group.
6. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, is characterized in that: an acidic catalyst in described step (1) is mineral acid or organic acid; Described mineral acid is HCl, H
2sO
4, H
3pO
4, H
2cO
3, HF, HBr, HNO
3, H
2sO
3or HClO
4one or more mixtures, described organic acid is CH
3cOOH, HOOC-COOH, HOOCC
2h
4cOOH or C
6h
5one or more mixtures of COOH.
7. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, is characterized in that: the organic solvent in described step (1) is one or more in methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol or acetone; Organic solvent in described step (3) is one or more of methyl alcohol, ethanol, ethylene glycol, propyl alcohol, propyl carbinol, isopropylcarbinol, Pentyl alcohol, primary isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol, acetone, butanone, normal hexane, isohexane, heptane or octane.
8. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, it is characterized in that: the dwell temperature in described step (2) is 20 ~ 80 DEG C, time of repose is 0.01 ~ 36 hour; Aging temperature is 30 ~ 80 DEG C, and the time is 0 ~ 48 hour.
9. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, it is characterized in that: the displacement temperature in described step (3) is 30 ~ 80 DEG C, the time is 1 ~ 36 hour, and number of times is 1 ~ 4 time.
10. the preparation method of hydrophobic type aerosil heat insulation composite material as claimed in claim 4, is characterized in that: the method for the drying in described step (4) is one or more in supercritical drying, constant pressure and dry, subcritical drying, vacuum-drying or lyophilize; The medium of described supercritical drying, subcritical drying is the one in carbonic acid gas, methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols, acetone or acetonitrile; Described constant pressure and dry temperature is 20 ~ 200 DEG C, and the time is 0.1 ~ 160h.
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