CN104231798B - Improved silica aerogel microball insulating moulding coating - Google Patents
Improved silica aerogel microball insulating moulding coating Download PDFInfo
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Abstract
Disclosed herein is a kind of insulating moulding coating using hydrophobic silicon dioxide aerogel microballoon as thermal insulating filling, key step includes, hydrophobic silica aerosil microballoon is first prepared, obtained silica aerosil microballoon and polymer emulsion are then mixed with insulating moulding coating.The hydrophobically modified of silica aerosil microballoon includes two ways, one kind is to be modified processing to silica wet gel microballoon using halogenated alkane, another method is, in colloidal sol preparatory phase, alkoxy silane, silazane or siloxanes to be added into mixed solution.Surfactant is added during coating preparation, is so conducive to increasing the compatibility between hydrophobic silica aerogel microballoon and polymer emulsion, dispersiveness of the microballoon in coating is improved, so as to improve the quality of coating, the heat-proof quality of coating is improved.
Description
Technical field
The present invention relates to a kind of novel heat-insulation coating using hydrophobic silicon dioxide aerogel microballoon as functional stuffing.Dioxy
SiClx aerogel microball is a kind of porous amorphous material with random three-dimensional network shape skeleton structure, using it mainly to fill out
Expect the insulating moulding coating light-weight environment-friendly prepared, density is low, and thermal insulation is good.Residential building, school, hospital are the composite can be widely applied to,
The inner-outer wall of the public buildings such as factory building and roof of storied building are heat-insulated, and the anti-heat expansion damage of the large volume such as bridge, dam building or facility is protected
Protect, the numerous areas such as protection that steamer, train, bus top are shown up day.
Background technology
Insulating moulding coating is by preventing the temperature of heat transfer, reduction coating and internal environment, so that improvement working environment is reached,
Reduce the purpose of energy consumption.Traditional insulating moulding coating is aggregate generally from functional stuffing, is combined together it by bonding agent, directly
Equipment or surface of wall formation layer protective layer is connected on to realize effect of insulation.It is commonly used for the heat-insulation and heat-preservation of functional stuffing
Material includes volcano gray glass, white jade stone, Black Warrior stone, sepiolite, bentonite, perlite, expanded vermiculite, calcium silicates etc., these
Material high temperature resistant, fire-retardant, compression strength is big, but their hygroscopicity is stronger, and expansion rate is larger, and weatherability is poor, is made with them
The coating shrinkage factor of main stuffing is big, crack resistance is poor, in order to form a stable heat insulation system, it is sometimes desirable to water layer of separately setting up defences
And external protection coating.
Silica aerosil microballoon is a kind of novel nano porous material of structure-controllable, its porosity 80%~
99%, specific surface area is up to 800-1000m2·g-1, average pore size is 1~50nm.It has thermal coefficient of expansion low, anti-oxidant,
Corrosion-resistant, extremely low the advantages of stability is good, wherein thermal conductivity factor are silica aerosil microballoon most outstanding features.It is conventional to protect
The thermal conductivity factor of adiabator is minimum up to 0.045W/mk, but the thermal conductivity factor of silica aerosil microballoon can reach
0.01W/mk, thus using silica aerosil microballoon for filler insulating moulding coating by be greatly enhanced insulating moulding coating every
Hot property.
The silica aerosil microballoon generally prepared has hydrophily, and substantial amounts of hydroxyl is contained on surface, and this causes them
The easy moisture absorption, meets water and crushes, while can also cause thermal conductivity factor to rise in atmosphere.The heat-insulated painting prepared by this aerogel microball
Expect that hygroscopicity is strong, weatherability is poor, with the extension of time, the thermal conductivity of coating rises, heat-proof quality drastically declines.
In order to improve the heat-proof quality of coating, the service life of coating is improved, it is necessary to which silica aerosil microballoon is entered
Row hydrophobically modified.Conventional method of modifying is to add modifying agent in the preparation process of silica aerosil microballoon at present.Often
Modifying agent includes trim,ethylchlorosilane, MTMS, HMDS, HMDS etc.,
These modifying agent carry alkyl, the hydrophobic grouping such as aryl or alkoxy, by introducing hydrophobic grouping to substitute microballoon table mostly
The hydroxyl in face is modified to silica aerosil microballoon.
Traditional coating includes oil paint and water paint.Oil paint usually contains many organic solvents and makees scattered be situated between
Matter, such as acetone, formaldehyde etc., these small-molecule substances enter the inside of silica aerosil microballoon or adsorbed micro- in aeroge
The surface of ball, will cause the rising of microballoon thermal conductivity factor.And water paint is with water as solvent or decentralized medium, while it is high to adulterate
Polymer emulsion is made in Molecularly Imprinted Polymer, as film forming matter, is very suitable for making the binding agent of silica aerosil microballoon, together
When water paint environmental protection, be the direction of following insulating moulding coating development.
There is extremely strong hydrophobicity by modified silica aerosil microballoon, surface tension is very big, add polymer
After emulsion, the mutually exclusive of interface will necessarily be produced, while microballoon is also difficult to form uniform scattered in coating, so that shadow
Ring the heat-proof quality of coating.In order to solve this problem, an effective method is that surfactant is added into coating.Surface
Activating agent is by two kinds of completely different molecular molecules of grain.Molecular structure has amphipathic, and lipophilic group, one are contained in one end
Contain hydrophilic radical in end.It can be aligned in the solution so that the surface tension of material is remarkably decreased in solution.Into coating
Minimal amount of surfactant is added, the interface phase between silica aerosil microballoon and polymeric binder is just obviously improved
Capacitive, prevents the cohesion between microballoon, greatly improves the quality of coating.
Silica aerosil microballoon carries out hydrophobically modified using modifying agent to wet gel in the present invention, obtains completely hydrophobic
Aerosil micron order bead.What is prepared by filler of the silica aerosil microballoon of this hydrophobically modified is heat-insulated
Coating, hygroscopicity is weak, and good weatherability, service life is long, while by adding surfactant in insulating moulding coating, being effectively improved
Interface state of the microballoon in coating and scattered situation so that the thermal conductivity of insulating moulding coating is reduced to 0.05W/mk, with city
Field like product is compared, and thermal insulation is more preferable.
The content of the invention
The invention provides a kind of novel heat-insulation painting using hydrophobically modified silica aerosil microballoon as thermal insulating filling
Material, this coating is main by polymeric binder, and silica aerosil microballoon, auxiliary agent adds surfactant mixing system simultaneously
Standby, dispersion stabilization is good, and thermal conductivity is low, the characteristics of with environmental protection and energy saving.
The technical solution adopted by the present invention is：
By selected silicon source and absolute ethyl alcohol, stirred after deionized water mixing, then add acid as catalyst, stirred,
Mixed solution is obtained, mixed solution is placed in water-bath, insulation a period of time, silicon dioxide gel is obtained；Silica is molten
Glue is sprayed into oil phase via atomizer, ensures lasting stirring in atomization process.By atomizer, silicon dioxide gel is with droplet
Form be injected into oil.Spread to ensure that obtained Wet Gel Microsphere uniformly divides, sol volume must not exceed oil phase volume
1/5.After the completion of atomization, ammoniacal liquor is added into mixed solution, at room temperature aging two days, obtain silica wet gel microballoon.
Silica wet gel microballoon is filtered, oil phase is filtered off, remaining oil phase and organic impurities is replaced using n-hexane, then with nothing
Water-ethanol replaces n-hexane, obtains pure silica wet gel microballoon；Hydrophobic treatment is carried out to wet gel with modifying agent；To
The mixed solution of deionized water and absolute ethyl alcohol is added in Wet Gel Microsphere after hydrophobic treatment, after cleaning modification
Foreign ion；Absolute ethyl alcohol, displacement wherein deionized water are added into Wet Gel Microsphere；Wet Gel Microsphere is dried.
Surfactant is mixed with polymer emulsion, auxiliary agent is added, stirs, dry two are added into mixed liquor
Silica aerogel microballoon, stirring adjusts viscosity, solidifies drying, obtains aerosil insulating moulding coating.
It is above-mentioned to prepare modifying agent used in aerosil for halogenated silanes, enumerate some types as follows：
a.X3Si(CnH2n+1) type and X3Si（CnH2n-1）Type Haloorganosilanes, X=Cl, Br, n=1-20.
b.X2(R')Si(CnH2n+1) type and X2(R')Si（CnH2n-1）Type Haloorganosilanes, X=Cl, Br, R'=such as examples
Such as methyl, ethyl, n-propyl, the alkyl or cycloalkyl of butyl, n=1-20.
c.X (R')2Si(CnH2n+1) type and X (R')2Si（CnH2n-1）Type Haloorganosilanes, X=Cl, Br, R'=is such as
Such as alkyl or cycloalkyl of methyl, ethyl, n-propyl, butyl, n=1-20.
d.X3Si(CH2) m-R' type Haloorganosilanes, X=Cl, Br, m=0.1-20, R'=methyl, aryl（Such as-C6H5,
Substituted phenyl）,-C4F9、-OCF2-CHF-CF3、-C6F13、-O-CF2-CHF2,-NH2、-N3、-SCN、-CH=CH2、-NH-CH2-
CH2-NH2、-N-(CH2-CH2-NH2)2、-OOC(CH3)C=CH2、-OCH2-CH(O)CH2、-NH-CO-N-CO-(CH2)、-NH-
COO-CH3、-NH-COO-CH2-CH3、NH-(NH2)3Si(OR)3、-SX-(CH2)3Si(OR)3、-SH
e.(R)X2Si(CH2)m- R' type Haloorganosilanes, X=Cl, Br, the alkyl of R=such as methyl, ethyl, propyl group,
M=0.1-20, R=methyl, aryl（Such as-C6H5, substituted phenyl）,-C4F9、-OCF2-CHF-CF3、-C6F13、-O-CF2-
CHF2,-NH2、-N3、-SCN、-CH=CH2、-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-OOC(CH3)C=CH2、-OCH2-
CH(O)CH2、-NH-CO-N-CO-(CH2)、-NH-COO-CH3、-NH-COO-CH2-CH3、NH-(NH2)3Si(OR)3(R therein
Base can be methyl, ethyl, propyl group, butyl) ,-SX-(CH2)3Si(OR)3(R bases therein can be methyl, ethyl, propyl group,
Butyl) ,-SH
f.(R)2XSi(CH2)m- R' type Haloorganosilanes, X=Cl, Br, m=0.1-20, R'=methyl, aryl（As-
C6H5, substituted phenyl）,-C4F9、-OCF2-CHF-CF3、-C6F13、-O-CF2-CHF2,-NH2、-N3、-SCN、-CH=CH2、-NH-
CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-OOC(CH3)C=CH2、-OCH2-CH(O)CH2、-NH-CO-N-CO-(CH2)、-
NH-COO-CH3、-NH-COO-CH2-CH3、NH-(NH2)3Si(OR)3、-SX-(CH2)3Si(OR)3、-SH。
Can be additionally that modifying agent carries out hydrophobically modified with alkoxy silane, silazane or siloxanes, using this modification
The technical scheme that agent prepares aerogel heat-proof coating is：
By silicon source, absolute ethyl alcohol, deionized water is mixed by a certain percentage, is stirred, and then adds acid as catalyst, is stirred
Mix uniform, obtain mixed liquor, mixed solution is placed in thermostat water bath, after insulation a period of time, add modifying agent, stirring is equal
It is even, then a period of time will be incubated in solution water-bath；Silicon dioxide gel is sprayed into oil phase by the way of atomization, atomization
During be kept stirring for state.By atomizer, silicon dioxide gel in the form of droplet to be present in oil.Atomization is completed
Afterwards, aging a couple of days, silica wet gel microballoon is obtained with adding ammoniacal liquor in the mixed solution of oil to colloidal sol；Filter off mixed liquor
In unnecessary oil phase, remaining oil and organic impurities is replaced using n-hexane, then n-hexane is replaced with absolute ethyl alcohol, obtains pure
Net silica wet gel microballoon, Wet Gel Microsphere is dried.
Auxiliary agent and surfactant are added in polymer emulsion, stirs, dry dioxy is added into mixed liquor
SiClx aerogel microball, stirring adjusts viscosity, solidifies drying, obtains aerosil insulating moulding coating.
Such modifying agent can be used alone or be used in mixed way, and its some types is as follows：
a.(RO)3Si(CnH2n+1) type and (RO)3Si(CnH2n-1) type organosilan, R=such as methyl, ethyl, positive third
Base, isopropyl, the silane of butyl, n=1-20
b.R'x(RO)ySi(CnH2n+1) type and (RO)3Si(CnH2n+1) type organosilan, the methyl of R=such as, ethyl,
N-propyl, isopropyl, the silane of butyl, the silane or cycloalkanes of R'=such as methyl, ethyl, n-propyl, isopropyl, butyl
Base, n=1-20, x+y=3, or x=1.2 or y=1.2
c.(RO)3Si(CH2)m- R' type organosilans, the alkyl of R=such as methyl, ethyl, propyl group, m=0.1-20, R'=first
Base, aryl（Such as-C6H5, substituted phenyl）,-C4F9、-OCF2-CHF-CF3、-C6F13、-O-CF2-CHF2,-NH2、-N3、-
SCN、-CH=CH2、-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-OOC(CH3)C=CH2、-OCH2-CH(O)CH2、-NH-
CO-N-CO-(CH2)、-NH-COO-CH3、-NH-COO-CH2-CH3、NH-(NH2)3Si(OR)3、-SX-(CH2)3Si(OR)3、-
SH ,-NR'R''R'''(R'=alkyl, aryl；R''=H, alkyl, aryl；R'''=H, alkyl, aryl, benzyl)
d.R'R2Si-N-SiR2(H) silazane of R ' types, R=alkyl, vinyl, aryl, R'=alkyl, vinyl, aryl
The cyclic polysilazane of e.D3, D4, D5 type, wherein D3, D4, D5 be with 3,4,5-O-Si (CH3)2The ring of-type
Shape polysiloxanes.
The silicon source that the present invention prepares used in silicon dioxide gel is silicate class（Including tetraethyl orthosilicate, methyl silicate
Deng）, Ludox and waterglass.Acid used includes nitric acid, hydrochloric acid, hydrofluoric acid, one or more of mixing therein such as oxalic acid.
Silicon source used, deionized water in the present invention, the mass fraction of absolute ethyl alcohol is respectively 10%~60%, 8%~72%,
25%~82%, acid is the catalyst of teos hydrolysis, and consumption is 1 ‰~the 4 ‰ of mixed liquor volume, and ammoniacal liquor is urged for gel
Agent, ammoniacal liquor content is mixed liquor volume 3 ‰~10 ‰.30 DEG C~90 DEG C, water bath time 0~6 day are kept in water-bath.
The oil phase that the present invention is used can select general plant blend oil, silicone oil etc., with certain viscosity.
Rotating speed used is 300r/min~2000r/min during present invention atomization.
Present invention cleaning remaining oil phase and organic impurities, n-hexane consumption are not less than the 1/10 of cleaning solution volume, often
Its cleaning 2~12 times, is cleaned 1~8 day.Washes of absolute alcohol n-hexane is used, ethanol consumption, which is not less than, cleans the 1/ of n-hexane
10, clean 2~12 times, clean 1~8 day daily.
Modifier content used of the invention is the 40%~180% of selected silicon source volume.
The present invention is when using halogenated silanes for modifying agent, with deionized water and the halogen that cleans after modifier treatment of mixed liquor
Race's ion, absolute ethyl alcohol is 1 with deionized water volume ratio:1~1:Cleaning in 10,1~5 days once, is cleaned 2~7 times altogether, cleaning
After the completion of, detected using silver nitrate solution, if precipitation, continue to clean.
The surfactant that the present invention is used primarily serves following effect:
1. promoting wetting of the polymer emulsion to hydrophobic silica aerogel microballoon, improve state of interface；
2. improve dispersiveness of the hydrophobic silica aerogel microballoon in coating；
3. improving the bin stability of coating, reduce and waste.
Surfactant of the invention used is divided into polymer dielectric class according to molecular structure, the poly- carboxylic acid of such as anion,
Calgon etc., inorganic polymeric alkali salt class, such as polycarboxylic acids ammonium salt, Diisobutylene maleic acid sodium salt etc., polyphosphazene polymer
Compound class, such as BYK-154（Acrylic polymer）, BYK-181（High-molecular block copolymer）Deng.
Binding agent of the invention used is polymer emulsion, such as epoxy resin, pure-acrylic emulsion, polyurethane etc., and coating used is helped
Agent is commercially available.Polymer emulsion accounts for the 10%~95% of coating cumulative volume, and the volume fraction of aerogel microball accounts for 5%~90%, table
Face active agent content is 0.1 ‰~the 5 ‰ of coating gross mass, and other auxiliary agent sums are no more than the 2 ‰ of coating quality.
The beneficial effect of insulating moulding coating prepared by the present invention：
Silica aerosil microballoon is light heat-insulating material, and thermal conductivity factor is filled out up to 0.01W/mk using it to be heat-insulated
The coating thermal insulation of material is good；Anticorrosive, anti-oxidant, the standby insulating moulding coating of water resistance pressure of hydrophobic silica aerogel microballoon
Hygroscopicity is poor, and washability, good weatherability, service life are long；The addition of surface-active, improves the interface state of coating, and dredge
Scattered situation of the water silica aerosil microballoon in coating, improves the physical property and heat-proof quality of coating.
Embodiment
Example 1
（1）It is prepared by silicon dioxide gel：Using 208.33g tetraethyl orthosilicate as silicon source, by tetraethyl orthosilicate with
92.14g absolute ethyl alcohols are mixed, and are stirred, and obtain mixed liquor 1.；Separately take 92.14g absolute ethyl alcohols and 72g deionized waters
Mixed, then add 2w% nitric acid 1ml, stir, obtain mixed liquor 2., by mixed liquor 1., be 2. mixed and stirred for 5
Minute or so, final mixed solution is obtained, mixed solution is placed in 60 DEG C of water-baths, two hours are incubated；
（2）The preparation of silica wet gel microballoon：Silicon dioxide gel imports atomizer by drainage tube, by 0.1mm
Atomizer nozzle immersion 500ml peanut oil in, peanut oil is kept stirring for state, opens atomizer switch.Protected in atomization process
Hold 800r/min mixing speed.By atomizer, silicon dioxide gel glue in the form of droplet to be injected into peanut oil.Note
The sol volume for entering peanut oil is 100ml.After the completion of atomization, 20w% ammoniacal liquor is added into the mixed solution of colloidal sol and peanut oil
3ml, aging two days, obtain silica wet gel microballoon at room temperature；
（3）The hydrophobically modified of Wet Gel Microsphere：By silica wet gel microballoon by filter tunnel, peanut oil is filtered off,
Remaining peanut oil and organic impurities is replaced using 150ml n-hexanes, 3 times a day, is replaced 3 days altogether, it is then anhydrous with 100ml
Ethanol replacement n-hexane, 3 times a day, replaces 3 days, obtains pure silica wet gel microballoon altogether；Use trimethylchloro-silicane
Alkane（Analysis is pure）To wet gel progress hydrophobic treatment, the volume ratio of trim,ethylchlorosilane and wet gel is 1:5, processing one in two days
It is secondary, modification 4 days；
（4）The drying of Wet Gel Microsphere：Into the Wet Gel Microsphere after hydrophobic treatment add deionized water with it is anhydrous
The volume ratio of the mixed solution of ethanol, the chlorion after cleaning trim,ethylchlorosilane processing, deionized water and absolute ethyl alcohol is 1:
1.Clean 3 times within one day, clean 3 days.Then detect whether also chlorion with 6w% silver nitrate solution, if precipitation, then after
Continuous cleaning.Ensure that chlorion is cleaned up, absolute ethyl alcohol, displacement wherein deionized water, daily 3 are added into Wet Gel Microsphere
It is secondary, replace 3 days altogether.Silica wet gel microballoon is dried at normal temperatures；
（5）The preparation of silica aerosil microballoon insulating moulding coating：By dispersant, wetting agent, defoamer, levelling agent etc. are helped
Agent is added in 20g pure-acrylic emulsions, is added anion surfactant sodium alkyl benzene sulfonate, is stirred, and is added into mixed liquor
Enter modified silica aerosil microballoon 6g, stir, add thickener regulation viscosity, obtain the heat-insulated painting of aerosil
Material.Auxiliary agent content is 0.01g, surface-active contents 0.01g；
（6）Thermal conductivity is detected using Hot disk TPS 2500S thermal conductivity coefficient measurement instruments, aerosil is micro-
The thermal conductivity of ball insulating moulding coating is 0.04866 W/ (mK).
Example 2
（1）It is prepared by silicon dioxide gel：Absolute ethyl alcohol is mixed by a certain percentage with deionized water, then to mixing
Liquid adds tetraethyl orthosilicate, wherein tetraethyl orthosilicate in me, deionized water, and the quality of absolute ethyl alcohol is respectively 208.33g, 72g,
322.49g, then adds 2w% nitric acid 1ml, stirs, obtain final mixed solution, mixed solution is placed in into 60 DEG C of water
In bath, two hours are incubated；
（2）The preparation of silica wet gel microballoon：Silicon dioxide gel imports atomizer by drainage tube, by 0.1mm
Atomizer nozzle immersion 500ml silicone oil in, silicone oil is kept stirring for state, opens atomizer switch.Kept in atomization process
900r/min mixing speed.By atomizer, silicon dioxide gel glue in the form of droplet to be present in silicone oil.Inject silicon
The sol volume of oil is 100ml.After the completion of atomization, 20w% ammoniacal liquor 3ml is added into the mixed solution of colloidal sol and silicone oil, in room
The lower aging of temperature two days, obtains silica wet gel microballoon；
（3）The hydrophobically modified of Wet Gel Microsphere：Filtering, filters off the silicone oil in mixed liquor, replaces remnants' using n-hexane
Silicone oil and organic impurities, 3 times a day, replace 3 days, then replace n-hexane with absolute ethyl alcohol, 3 times a day, 3 are replaced altogether altogether
My god, obtain pure silica wet gel microballoon；Use trim,ethylchlorosilane（Analysis is pure）Hydrophobic treatment, three are carried out to wet gel
The volume ratio of methylchlorosilane and wet gel is 1:5, handle once within two days, modification 4 days；
（4）The drying of Wet Gel Microsphere：Into the Wet Gel Microsphere after hydrophobic treatment add deionized water with it is anhydrous
The mixed solution of ethanol, the chlorion after cleaning trim,ethylchlorosilane processing, the volume of deionized water and absolute ethyl alcohol is
400ml is cleaned 3 times for mono- day, is cleaned 3 days.Then also chlorion is detected whether with 6w% silver nitrate solution, if precipitation,
Then continue to clean.After ensuring that chlorion is cleaned up, absolute ethyl alcohol is added into Wet Gel Microsphere, wherein deionized water is replaced,
Absolute ethyl alcohol consumption is 150ml, 3 times a day, is replaced 3 days altogether.Wet Gel Microsphere is entered using supercritical carbon dioxide device
Row drying；
（5）The preparation of aerogel heat-proof coating：By cetyl trimethyl chlorine（Bromine）Change ammonium（Cationic surfactant
1631）Same dispersant, wetting agent, the auxiliary agent such as defoamer, levelling agent are added in 20g epoxy resin latexes, surfactant and are helped
Agent content is 0.01g, is stirred, and modified silica aerosil microballoon 6g is added into mixed liquor, is stirred, and is added
0.01g thickeners adjust viscosity, stir 3 minutes, add 2g curing agent, and stirring is dried at room temperature for solidification three days, obtains dioxy
SiClx aerogel heat-proof coating；
（6）Thermal conductivity is detected using Hot disk TPS 2500S thermal conductivity coefficient measurement instruments, aerosil is micro-
The thermal conductivity of ball insulating moulding coating is 0.06098 W/ (mK).
Example 3
（1）It is prepared by silicon dioxide gel：By 460.7g absolute ethyl alcohols and 72g deionized water by being mixed, Ran Houxiang
288.33g tetraethyl orthosilicates are added in mixed liquor, 2w% nitric acid 1ml is then added, stirs, mixed solution is placed in 60
In DEG C water-bath, 118.62g dimethyldiethoxysilanes are added in 8 minutes backward mixed liquors, by mixed liquor in insulation two
Hour；
（2）The preparation of silica wet gel microballoon：Silicon dioxide gel introduces atomizer by drainage tube, uses
0.3mm atomizer nozzle.Using peanut oil as oil phase, peanut oil 800r/min rotating speed is kept, silicon dioxide gel is sprayed into
In peanut oil.800r/min mixing speed is kept in atomization process.The sol volume sprayed into 500ml peanut oil is
100ml.After the completion of atomization, 20w% ammoniacal liquor 3ml is added into the mixed liquor of colloidal sol and peanut oil, at room temperature aging two days,
Obtain silica wet gel microballoon；
（3）The drying of Wet Gel Microsphere：Filtering, filters off the peanut oil in mixed liquor, and remaining oil is replaced using n-hexane
And organic impurities, 3 times a day, replace altogether 3 days, then replace n-hexane with absolute ethyl alcohol, 3 times a day, replace 3 days altogether,
Obtain pure silica wet gel microballoon.Wet Gel Microsphere is dried using Supercritical Ethanol device；
（4）The preparation of aerogel heat-proof coating：Surface is used as using 0.015g fatty acid methyl ester APEO FMEE
Activating agent, by its dispersant, wetting agent with 0.01g, the auxiliary agent such as defoamer, levelling agent is added in 20g epoxy resin latexes, stirred
Mix uniform, then add modified silica aerosil microballoon 5g, stir, add 0.01g thickeners regulation viscosity, stirring 3
Minute, solidification three days is dried at room temperature for, aerosil insulating moulding coating is obtained；
（5）Thermal conductivity is detected using Hot disk TPS 2500S thermal conductivity coefficient measurement instruments, aerosil is micro-
The thermal conductivity of ball insulating moulding coating is 0.06980 W/ (mK).
Claims (1)
1. a kind of preparation method of hydrophobic silica aerogel microsphere insulating coating, it is characterised in that：The preparation method is
Realized by following step：
（1）It is prepared by silicon dioxide gel：Using 208.33g tetraethyl orthosilicate as silicon source, by tetraethyl orthosilicate and 92.14g without
Water-ethanol is mixed, and is stirred, and obtains mixed liquor 1.；Separately 92.14g absolute ethyl alcohols are taken to be mixed with 72g deionized waters,
Then 2w% nitric acid 1ml is added, stirs, obtains mixed liquor 2., 1., 2. mixed liquor is mixed and stirred for 5 minutes or so,
Final mixed solution is obtained, mixed solution is placed in 60 DEG C of water-baths, two hours are incubated；
（2）The preparation of silica wet gel microballoon：Silicon dioxide gel imports atomizer by drainage tube, by 0.1mm mist
Change in device nozzle immersion 500ml peanut oil, peanut oil is kept stirring for state, open and kept in atomizer switch, atomization process
800r/min mixing speed, by atomizer, silicon dioxide gel glue is injected with being injected into the form of droplet in peanut oil
The sol volume of peanut oil is 100ml, after the completion of atomization, and 20w% ammoniacal liquor is added into the mixed solution of colloidal sol and peanut oil
3ml, aging two days, obtain silica wet gel microballoon at room temperature；
（3）The hydrophobically modified of Wet Gel Microsphere：By silica wet gel microballoon by filter tunnel, peanut oil is filtered off, every time
Remaining peanut oil and organic impurities is replaced using 150ml n-hexanes, 3 times a day, replaces 3 days altogether, 100ml is then used every time
Absolute ethyl alcohol replaces n-hexane, 3 times a day, replaces 3 days altogether, obtains pure silica wet gel microballoon；Use trimethyl
Chlorosilane carries out hydrophobic treatment to Wet Gel Microsphere, and the volume ratio of trim,ethylchlorosilane and Wet Gel Microsphere is 1:5, handle within two days
Once, modification 4 days；
（4）The drying of Wet Gel Microsphere：Deionized water and absolute ethyl alcohol are added into the Wet Gel Microsphere after hydrophobic treatment
Mixed solution, the chlorion after cleaning trim,ethylchlorosilane processing, the volume ratio of deionized water and absolute ethyl alcohol is 1:1, one
Its cleaning 3 times, cleans 3 days, then detects whether also chlorion with 6w% silver nitrate solution, if precipitation, then continues clear
Wash, it is ensured that chlorion is cleaned up, absolute ethyl alcohol is added into Wet Gel Microsphere, replace wherein deionized water, 3 times a day, always
Replace 3 days altogether, silica wet gel microballoon is dried at normal temperatures, obtains modified silica aerosil microballoon；
（5）The preparation of silica aerosil microballoon insulating moulding coating：By dispersant, wetting agent, each 0.01g of defoamer, levelling agent
Add in 20g pure-acrylic emulsions, add 0.01g anion surfactant sodium alkyl benzene sulfonates, stir, into mixed liquor
Add step（4）The silica aerosil microballoon 6g of obtained modification, stirring adds thickener regulation viscosity, obtains dioxy
SiClx aerogel heat-proof coating, is detected, silica using Hot disk TPS 2500S thermal conductivity coefficient measurement instruments to thermal conductivity
The thermal conductivity of aerogel microball insulating moulding coating is 0.04866 W/ (mK).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310242852.7A CN104231798B (en) | 2013-06-19 | 2013-06-19 | Improved silica aerogel microball insulating moulding coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310242852.7A CN104231798B (en) | 2013-06-19 | 2013-06-19 | Improved silica aerogel microball insulating moulding coating |
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| RU2011148097A (en) * | 2009-04-27 | 2013-06-10 | Роквул Интернэшнл А/С | AEROGEL GEL COMPOSITIONS AND METHODS FOR THEIR MANUFACTURE AND USE |
| US20120142240A1 (en) * | 2010-12-07 | 2012-06-07 | Basf Se | Polyurethane composite material |
| CN102604468B (en) * | 2012-02-03 | 2014-06-25 | 广州泰祥混凝土外加剂有限公司 | SiO2 aerogel thermal insulation latex paint and preparation method thereof |
| CN102719129B (en) * | 2012-07-05 | 2013-08-21 | 河南工业大学 | Preparation method of silica aerogel aqueous heat-insulating coating |
| CN102838933B (en) * | 2012-09-27 | 2015-09-16 | 富思特新材料科技发展股份有限公司 | Self-cleaning heat-insulation coating and preparation method thereof |
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