CN104231798A - Modified silicon dioxide aerogel microsphere thermal-insulation coating - Google Patents
Modified silicon dioxide aerogel microsphere thermal-insulation coating Download PDFInfo
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- CN104231798A CN104231798A CN201310242852.7A CN201310242852A CN104231798A CN 104231798 A CN104231798 A CN 104231798A CN 201310242852 A CN201310242852 A CN 201310242852A CN 104231798 A CN104231798 A CN 104231798A
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Abstract
The invention discloses a thermal-insulation coating by taking hydrophobic silicon dioxide aerogel microspheres as thermal-insulation packing. The coating is prepared by the following main steps: preparing the hydrophobic silicon dioxide aerogel microspheres; and mixing the prepared hydrophobic silicon dioxide aerogel microspheres and a polymer emulsion to prepare the thermal-insulation coating. Hydrophobic modification of the silicon dioxide aerogel microspheres includes the following two modes: in one mode, silicon dioxide wet-gel microspheres are modified by adopting halogenated hydrocarbon and in the other mode, alkoxy silane, silazane or siloxane is added into a mixed solution in a sol preparing stage. When the coating is prepared, a surfactant is added, so that the compatibility between the hydrophobic silicon dioxide aerogel microspheres and the polymer emulsion can be improved, the dispersibility of the microspheres in the coating can be improved, the coating quality can be improved, and the thermal-insulation performance of the coating can be improved.
Description
Technical field
The present invention relates to a kind of novel heat-insulation coating being functional stuffing with hydrophobic silicon dioxide aerogel microballoon.Silica aerosil microballoon is a kind of porous amorphous material with random three-dimensional network shape skeleton structure, and the thermal insulating coating light-weight environment-friendly prepared for main stuffing with it, density is low, and thermal insulation is good.The present invention can be widely used in residential building, school, hospital; inner-outer wall and the roof of storied building of the public buildings such as factory building are heat insulation; the anti-heat expansion injury protection of the large volume such as bridge, dam building or facility, the numerous areas such as the protection that steamer, train, bus top day show up.
Background technology
Thermal insulating coating, by stoping thermal conduction, reduces the temperature of coating and internal medium, thus reaches and improve Working environment, reduces the object of energy consumption.Tradition thermal insulating coating selects functional stuffing to be aggregate usually, relies on caking agent to make it combine, and directly forms at equipment or surface of wall effect that layer protective layer realizes heat insulating.The heat-insulating heat-preserving material being commonly used for functional stuffing comprises volcanic ash glass, white jade stone, Black Warrior stone, sepiolite, wilkinite, perlite, expanded vermiculite, Calucium Silicate powder etc., these materials are high temperature resistant, fire-retardant, ultimate compression strength is large, but their water absorbability is comparatively strong, and rate of expansion is larger, weathering resistance is poor, doing with them that the coating shrinking percentage of main stuffing is large, splitting resistance is poor, in order to form a stable heat insulation system, sometimes needing separately set up defences water layer and external protection coating.
Silica aerosil microballoon is a kind of novel nano porous material of structure-controllable, and its porosity is 80% ~ 99%, and specific surface area is up to 800-1000m
2g
-1, mean pore size is 1 ~ 50nm.It is low that it has thermal expansivity, anti-oxidant, corrosion-resistant, the advantages such as good stability, and wherein thermal conductivity is extremely low is the most outstanding feature of silica aerosil microballoon.The thermal conductivity of conventional lagging material is minimum reaches 0.045W/mk, but the thermal conductivity of silica aerosil microballoon can reach 0.01W/mk, the thermal insulating coating therefore utilizing silica aerosil microballoon to be filler will greatly improve the heat-proof quality of thermal insulating coating.
The silica aerosil microballoon of usual preparation has wetting ability, and surface is containing a large amount of hydroxyls, and this makes their the easy moisture absorption in atmosphere, meets water fragmentation, thermal conductivity also can be made to increase simultaneously.The thermal insulating coating water absorbability prepared by this aerogel microball is strong, and weathering resistance is poor, and along with the prolongation of time, the thermal conductivity of coating rises, and heat-proof quality sharply declines.
In order to improve the heat-proof quality of coating, improving the work-ing life of coating, hydrophobically modified must be carried out to silica aerosil microballoon.Method of modifying conventional at present adds properties-correcting agent in the preparation process of silica aerosil microballoon.Conventional properties-correcting agent comprises trimethylchlorosilane, methyltrimethoxy silane, hexamethyldisilazane, hexamethyldisilazane etc., these properties-correcting agent are mostly with alkyl, the hydrophobic grouping such as aryl or alkoxyl group, carries out modification with the hydroxyl of alternative microsphere surface to silica aerosil microballoon by introducing hydrophobic grouping.
Traditional coating comprises oil paint and water-borne coatings.Oil paint makes dispersion medium containing many organic solvents usually, and as acetone, formaldehyde etc., these small-molecule substances enter the inside of silica aerosil microballoon or are adsorbed on the surface of aerogel microball, will cause the rising of microballoon thermal conductivity.And water-borne coatings is with water as solvent or dispersion medium, polymer emulsion made by the high molecular polymer that simultaneously adulterates, and as filmogen, is very suitable for the binding agent making silica aerosil microballoon, water-borne coatings environmental protection is simultaneously the direction of following thermal insulating coating development.
Silica aerosil microballoon through modification has extremely strong hydrophobicity, surface tension is very large, after adding polymer emulsion, will inevitably produce the mutual repulsion at interface, microballoon is also difficult in coating, form uniform dispersion simultaneously, thus affects the heat-proof quality of coating.In order to address this problem, an effective way adds tensio-active agent in coating.Tensio-active agent is by distinct two kinds of molecular molecules of grain.Molecular structure has amphipathic, and lipophilic group is contained in one end, and hydrophilic radical is contained in one end.It can align in the solution, and the surface tension of material in solution is significantly declined.In coating, add the tensio-active agent of minute quantity, just obviously improve the interface compatibility between silica aerosil microballoon and polymeric binder, prevent the cohesion between microballoon, significantly improve the quality of coating.
In the present invention, silica aerosil microballoon adopts properties-correcting agent to carry out hydrophobically modified to wet gel, obtains completely hydrophobic aerosil micron order bead.With the thermal insulating coating that the silica aerosil microballoon of this hydrophobically modified is prepared for filler, water absorbability is weak, good weatherability, long service life, simultaneously by adding tensio-active agent in thermal insulating coating, effectively improve the interfacial state of microballoon in coating and dispersion situation, make the thermal conductivity of thermal insulating coating be reduced to 0.05W/mk, compared with the like product of market, thermal insulation is better.
Summary of the invention
The invention provides a kind of novel heat-insulation coating using hydrophobically modified silica aerosil microballoon as thermal insulating filling, this coating is primarily of polymeric binder, silica aerosil microballoon, auxiliary agent adds tensio-active agent simultaneously and is mixed with, dispersion stabilization is good, thermal conductivity is low, has the feature of environmental protection and energy saving.
The technical solution used in the present invention is:
By selected silicon source and dehydrated alcohol, stir after deionized water mixing, then add acid as catalyst, stir, obtain mixing solutions, mixing solutions is placed in water-bath, insulation for some time, obtain silicon dioxide gel; Silicon dioxide gel sprays in oil phase via spraying gun, ensures Keep agitation in atomization process.By spraying gun, silicon dioxide gel is injected in oil with the form of small droplets.Spread to ensure that the Wet Gel Microsphere obtained evenly divides, sol volume must not exceed 1/5 of oil phase volume.After being atomized, in mixing solutions, add ammoniacal liquor, at room temperature aging two days, obtain silica wet gel microballoon.Filtered by silica wet gel microballoon, elimination oil phase, the oil phase adopting normal hexane displacement remaining and organic impurity, then replace normal hexane with dehydrated alcohol, obtain pure silica wet gel microballoon; With properties-correcting agent, hydrophobic treatment is carried out to wet gel; The mixing solutions of deionized water and dehydrated alcohol is added, the foreign ion after cleaning modification in the Wet Gel Microsphere after hydrophobic treatment; In Wet Gel Microsphere, add dehydrated alcohol, replace wherein deionized water; Drying is carried out to Wet Gel Microsphere.
Mixed with polymer emulsion by tensio-active agent, add auxiliary agent, stir, add dry silica aerosil microballoon in mixed solution, stir, adjusting viscosity, solidification is dry, obtains aerosil thermal insulating coating.
Above-mentioned to prepare aerosil properties-correcting agent used be halogenated silanes, enumerates some types as follows:
A. X
3si (C
nh
2n+1) type and X
3si(C
nh
2n-1) type Haloorganosilanes, X=Cl, Br, n=1-20.
B. X
2(R') Si (C
nh
2n+1) type and X
2(R') Si(C
nh
2n-1) type Haloorganosilanes, X=Cl, Br, the alkyl or cycloalkyl of R'=such as such as methyl, ethyl, n-propyl, butyl, n=1-20.
C. X (R')
2si (C
nh
2n+1) type and X (R')
2si(C
nh
2n-1) type Haloorganosilanes, X=Cl, Br, the alkyl or cycloalkyl of R'=such as such as methyl, ethyl, n-propyl, butyl, n=1-20.
D. X
3si (CH
2) m-R' type Haloorganosilanes, X=Cl, Br, m=0.1-20, R'=methyl, aryl are (as-C
6h
5, the phenyl of replacement) ,-C
4f
9,-OCF
2-CHF-CF
3,-C
6f
13,-O-CF
2-CHF
2,-NH
2,-N
3,-SCN ,-CH=CH
2,-NH-CH
2-CH
2-NH
2,-N-(CH
2-CH
2-NH
2)
2,-OOC (CH
3) C=CH
2,-OCH
2-CH (O) CH
2,-NH-CO-N-CO-(CH
2) ,-NH-COO-CH
3,-NH-COO-CH
2-CH
3, NH-(NH
2)
3si (OR)
3,-S
x-(CH
2)
3si (OR)
3,-SH
E. (R) X
2si (CH
2)
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-C
6h
5, the phenyl of replacement) ,-C
4f
9,-OCF
2-CHF-CF
3,-C
6f
13,-O-CF
2-CHF
2,-NH
2,-N
3,-SCN ,-CH=CH
2,-NH-CH
2-CH
2-NH
2,-N-(CH
2-CH
2-NH
2)
2,-OOC (CH
3) C=CH
2,-OCH
2-CH (O) CH
2,-NH-CO-N-CO-(CH
2) ,-NH-COO-CH
3,-NH-COO-CH
2-CH
3, NH-(NH
2)
3si (OR)
3(R base wherein can be methyl, ethyl, propyl group, butyl) ,-S
x-(CH
2)
3si (OR)
3(R base wherein can be methyl, ethyl, propyl group, butyl) ,-SH
F. (R)
2xSi (CH
2)
m-R' type Haloorganosilanes, X=Cl, Br, m=0.1-20, R'=methyl, aryl are (as-C
6h
5, the phenyl of replacement) ,-C
4f
9,-OCF
2-CHF-CF
3,-C
6f
13,-O-CF
2-CHF
2,-NH
2,-N
3,-SCN ,-CH=CH
2,-NH-CH
2-CH
2-NH
2,-N-(CH
2-CH
2-NH
2)
2,-OOC (CH
3) C=CH
2,-OCH
2-CH (O) CH
2,-NH-CO-N-CO-(CH
2) ,-NH-COO-CH
3,-NH-COO-CH
2-CH
3, NH-(NH
2)
3si (OR)
3,-S
x-(CH
2)
3si (OR)
3,-SH.
Useful alkoxy radicals silane, silazane or siloxanes are that properties-correcting agent carries out hydrophobically modified in addition, and the technical scheme adopting this properties-correcting agent to prepare aerogel heat-proof coating is:
By silicon source, dehydrated alcohol, deionized water mixes by a certain percentage, stirs, then acid as catalyst is added, stir, obtain mixed solution, mixing solutions is placed in thermostat water bath, after insulation for some time, add properties-correcting agent, stir, be then incubated for some time by solution water bath; Adopt the mode of atomization to spray in oil phase by silicon dioxide gel, in atomization process, keep whipped state.By spraying gun, silicon dioxide gel is present in oil with the form of small droplets.After being atomized, in colloidal sol and oily mixing solutions, adding ammoniacal liquor, aging a couple of days, obtain silica wet gel microballoon; Oil phase unnecessary in elimination mixed solution, the oil adopting normal hexane displacement remaining and organic impurity, then replace normal hexane with dehydrated alcohol, obtain pure silica wet gel microballoon, carry out drying to Wet Gel Microsphere.
Add in polymer emulsion by auxiliary agent and tensio-active agent, stir, add dry silica aerosil microballoon in mixed solution, stir, adjusting viscosity, solidification is dry, obtains aerosil thermal insulating coating.
This type of properties-correcting agent can be used alone or used in combination, and its some types is as follows:
A. (RO)
3si (C
nh
2n+1) type and (RO)
3si (C
nh
2n-1) type organosilane, the silane of R=such as such as methyl, ethyl, n-propyl, sec.-propyl, butyl, n=1-20
B. R'
x(RO)
ysi (C
nh
2n+1) type and (RO)
3si (C
nh
2n+1) type organosilane, the silane of R=such as such as methyl, ethyl, n-propyl, sec.-propyl, butyl, the silane of R'=such as such as methyl, ethyl, n-propyl, sec.-propyl, butyl or cycloalkyl, n=1-20, x+y=3, or x=1.2 or y=1.2
C. (RO)
3si (CH
2)
m-R' type organosilane, the alkyl of R=such as methyl, ethyl, propyl group, m=0.1-20, R'=methyl, aryl are (as-C
6h
5, the phenyl of replacement) ,-C
4f
9,-OCF
2-CHF-CF
3,-C
6f
13,-O-CF
2-CHF
2,-NH
2,-N
3,-SCN ,-CH=CH
2,-NH-CH
2-CH
2-NH
2,-N-(CH
2-CH
2-NH
2)
2,-OOC (CH
3) C=CH
2,-OCH
2-CH (O) CH
2,-NH-CO-N-CO-(CH
2) ,-NH-COO-CH
3,-NH-COO-CH
2-CH
3, NH-(NH
2)
3si (OR)
3,-S
x-(CH
2)
3si (OR)
3,-SH ,-NR'R''R'''(R'=alkyl, aryl; R''=H, alkyl, aryl; R'''=H, alkyl, aryl, benzyl)
D. R'R
2si-N-SiR
2(H) silazane of R ' type, R=alkyl, vinyl, aryl, R'=alkyl, vinyl, aryl
E. the cyclic polysilazane of D3, D4, D5 type, wherein D3, D4, D5 are with 3,4,5-O-Si (CH
3)
2the cyclic polysiloxanes of-type.
It is silicate class (comprising tetraethoxy, methyl silicate etc.), silicon sol and water glass that the present invention prepares silicon dioxide gel silicon source used.Acid used comprises nitric acid, hydrochloric acid, hydrofluoric acid, the mixing of wherein one or more such as oxalic acid.
Silicon source used in the present invention, deionized water, the massfraction of dehydrated alcohol is respectively 10% ~ 60%, 8% ~ 72%, 25% ~ 82%, acid is the catalyzer of teos hydrolysis, and consumption is 1 ‰ ~ 4 ‰ of mixed liquor volume, ammoniacal liquor is gel catalyst, and ammoniacal liquor content is mixed liquor volume 3 ‰ ~ 10 ‰.30 DEG C ~ 90 DEG C are kept, water bath time 0 ~ 6 day in water-bath.
The oil phase that the present invention adopts can select general plant blend oil, silicone oil etc., has certain viscosity.
When the present invention is atomized, rotating speed used is 300r/min ~ 2000r/min.
The oil phase of erase residual of the present invention and organic impurity, normal hexane consumption is not less than 1/10 of cleaning solution volume, cleans 2 ~ 12 every day, cleans 1 ~ 8 day.Use washes of absolute alcohol normal hexane, ethanol consumption is not less than 1/10 of cleaned normal hexane, cleans 2 ~ 12 every day, cleans 1 ~ 8 day.
The present invention's modifier content used is 40% ~ 180% of selected silicon volume source.
When the present invention adopts halogenated silanes to be properties-correcting agent, with deionized water and mixed solution clean the halogen family ion after modifier treatment, dehydrated alcohol and deionized water volume ratio are 1:1 ~ 1:10, cleaning in 1 ~ 5 day once, altogether clean 2 ~ 7 times, after having cleaned, adopt silver nitrate solution to detect, if there is precipitation, continue cleaning.
The tensio-active agent that the present invention adopts mainly functions as follows:
1. promote polymer emulsion soaking hydrophobic silica aerogel microballoon, improve state of interface;
2. improve the dispersiveness of hydrophobic silica aerogel microballoon in coating;
3. improve the package stability of coating, cut the waste.
The present invention's tensio-active agent used is divided into polymer dielectric class according to molecular structure, as negatively charged ion gathers carboxylic acid, Sodium hexametaphosphate 99 etc., inorganic polymeric alkali salt class, as poly carboxylic acid ammonium salt, Diisobutylene maleic acid sodium salt etc., high molecular polymer class, as BYK-154(acrylic polymer), BYK-181(high-molecular block copolymer) etc.
The present invention's binding agent used is polymer emulsion, and as epoxy resin, pure-acrylic emulsion, urethane etc., coatings additive(s) used is commercially available.Polymer emulsion accounts for 10% ~ 95% of coating cumulative volume, and the volume fraction of aerogel microball accounts for 5% ~ 90%, and surfactant content is 0.1 ‰ ~ 5 ‰ of coating total mass, and other auxiliary agent sums are no more than 2 ‰ of coating quality.
The beneficial effect of the thermal insulating coating prepared by the present invention:
Silica aerosil microballoon is light heat-insulating material, and thermal conductivity can reach 0.01W/mk, and the coating thermal insulation being thermal insulating filling with it is good; Hydrophobic silica aerogel microballoon anticorrosive, anti-oxidant, water tolerance forces standby thermal insulating coating water absorbability poor, washability, good weatherability, long service life; Surface-active interpolation, improves the interfacial state of coating, and the dispersion situation of hydrophobic silica aerogel microballoon in coating, improves physicals and the heat-proof quality of coating.
Embodiment
Example 1
(1) silicon dioxide gel preparation: using the tetraethoxy of 208.33g as silicon source, tetraethoxy is mixed with 92.14g dehydrated alcohol, stirs, obtain mixed solution 1.; Separately get 92.14g dehydrated alcohol to mix with 72g deionized water, then add the nitric acid 1ml of 2w%, stir, obtain mixed solution 2., 1., 2. mixed solution mixed and stirs about 5 minutes, obtaining final mixing solutions, mixing solutions is placed in 60 DEG C of water-baths, is incubated two hours;
(2) preparation of silica wet gel microballoon: silicon dioxide gel imports spraying gun by drainage tube, immersed by the atomizer nozzle of 0.1mm in 500ml peanut oil, peanut oil keeps whipped state, opens spraying gun switch.The stirring velocity of 800r/min is kept in atomization process.By spraying gun, silicon dioxide gel glue is injected in peanut oil with the form of small droplets.The sol volume injecting peanut oil is 100ml.After being atomized, in the mixing solutions of colloidal sol and peanut oil, adding the ammoniacal liquor 3ml of 20w%, at room temperature aging two days, obtain silica wet gel microballoon;
(3) hydrophobically modified of Wet Gel Microsphere: silica wet gel microballoon is passed through filter funnel, elimination peanut oil, the peanut oil adopting the displacement of 150ml normal hexane remaining and organic impurity, every day 3 times, altogether replace 3 days, then with 100ml dehydrated alcohol displacement normal hexane, every day 3 times, altogether replace 3 days, obtain pure silica wet gel microballoon; Carry out hydrophobic treatment with trimethylchlorosilane (analytical pure) to wet gel, the volume ratio of trimethylchlorosilane and wet gel is 1:5, within two days, processes once, modification 4 days;
(4) drying of Wet Gel Microsphere: the mixing solutions adding deionized water and dehydrated alcohol in the Wet Gel Microsphere after hydrophobic treatment, the chlorion after the process of cleaning trimethylchlorosilane, the volume ratio of deionized water and dehydrated alcohol is 1:1.Cleaning in one day 3 times, cleans 3 days.Then detect whether also have chlorion with the silver nitrate solution of 6w%, if there is precipitation, then continue cleaning.Guarantee that chlorion cleans up, in Wet Gel Microsphere, add dehydrated alcohol, replace wherein deionized water, every day 3 times, altogether replace 3 days.Silica wet gel microballoon carries out drying at normal temperatures;
(5) preparation of silica aerosil microballoon thermal insulating coating: by dispersion agent, wetting agent, the auxiliary agent such as defoamer, flow agent adds in 20g pure-acrylic emulsion, add anion surfactant sodium alkyl benzene sulfonate again, stir, the silica aerosil microballoon 6g of modification is added in mixed solution, stir, add thickening material adjusting viscosity, obtain aerosil thermal insulating coating.Auxiliary agent content is 0.01g, surfactant content 0.01g;
(6) adopt Hot disk TPS 2500S thermal conductivity coefficient measurement instrument to detect thermal conductivity, the thermal conductivity of silica aerosil microballoon thermal insulating coating is 0.04866 W/ (mK).
Example 2
(1) silicon dioxide gel preparation: dehydrated alcohol is mixed by a certain percentage with deionized water, then tetraethoxy is added, wherein tetraethoxy, deionized water to mixed solution in me, the quality of dehydrated alcohol is respectively 208.33g, 72g, 322.49g, then add the nitric acid 1ml of 2w%, stir, obtain final mixing solutions, mixing solutions is placed in 60 DEG C of water-baths, be incubated two hours;
(2) preparation of silica wet gel microballoon: silicon dioxide gel imports spraying gun by drainage tube, immersed by the atomizer nozzle of 0.1mm in 500ml silicone oil, silicone oil keeps whipped state, opens spraying gun switch.The stirring velocity of 900r/min is kept in atomization process.By spraying gun, silicon dioxide gel glue is present in silicone oil with the form of small droplets.The sol volume injecting silicone oil is 100ml.After being atomized, in the mixing solutions of colloidal sol and silicone oil, adding the ammoniacal liquor 3ml of 20w%, at room temperature aging two days, obtain silica wet gel microballoon;
(3) hydrophobically modified of Wet Gel Microsphere: filter, silicone oil in elimination mixed solution, the silicone oil adopting normal hexane displacement remaining and organic impurity, every day 3 times, altogether replace 3 days, then replace normal hexane with dehydrated alcohol, every day 3 times, altogether replace 3 days, obtain pure silica wet gel microballoon; Carry out hydrophobic treatment with trimethylchlorosilane (analytical pure) to wet gel, the volume ratio of trimethylchlorosilane and wet gel is 1:5, within two days, processes once, modification 4 days;
(4) drying of Wet Gel Microsphere: the mixing solutions adding deionized water and dehydrated alcohol in the Wet Gel Microsphere after hydrophobic treatment, chlorion after the process of cleaning trimethylchlorosilane, the volume of deionized water and dehydrated alcohol is 400ml and cleans 3 times in mono-day, cleans 3 days.Then detect whether also have chlorion with the silver nitrate solution of 6w%, if there is precipitation, then continue cleaning.After guaranteeing that chlorion cleans up, in Wet Gel Microsphere, add dehydrated alcohol, replace wherein deionized water, dehydrated alcohol consumption is 150ml, every day 3 times, altogether replaces 3 days.Supercritical co device is adopted to carry out drying to Wet Gel Microsphere;
(5) preparation of aerogel heat-proof coating: cetyl trimethyl chlorine (bromine) is changed ammonium (cats product 1631) same to dispersion agent, wetting agent, the auxiliary agent such as defoamer, flow agent adds in 20g epoxy resin latex, tensio-active agent and auxiliary agent content are 0.01g, stir, the silica aerosil microballoon 6g of modification is added in mixed solution, stir, add 0.01g thickening material adjusting viscosity, stir 3 minutes, add 2g solidifying agent, stir, at room temperature dry solidification three days, obtains aerosil thermal insulating coating;
(6) adopt Hot disk TPS 2500S thermal conductivity coefficient measurement instrument to detect thermal conductivity, the thermal conductivity of silica aerosil microballoon thermal insulating coating is 0.06098 W/ (mK).
Example 3
(1) silicon dioxide gel preparation: by the deionized water of 460.7g dehydrated alcohol and 72g by mixing, then in mixed solution, 288.33g tetraethoxy is added, then the nitric acid 1ml of 2w% is added, stir, mixing solutions is placed in 60 DEG C of water-baths, 118.62g dimethyldiethoxysilane is added, by mixed solution insulation two hours in 8 minutes backward mixed solutions;
(2) preparation of silica wet gel microballoon: silicon dioxide gel introduces spraying gun by drainage tube, adopts the atomizer nozzle of 0.3mm.Take peanut oil as oil phase, keep the rotating speed of peanut oil 800r/min, silicon dioxide gel is sprayed in peanut oil.The stirring velocity of 800r/min is kept in atomization process.The sol volume sprayed in 500ml peanut oil is 100ml.After being atomized, in the mixed solution of colloidal sol and peanut oil, adding the ammoniacal liquor 3ml of 20w%, at room temperature aging two days, obtain silica wet gel microballoon;
(3) drying of Wet Gel Microsphere: filter, peanut oil in elimination mixed solution, the oil adopting normal hexane displacement remaining and organic impurity, every day 3 times, altogether replace 3 days, then replace normal hexane with dehydrated alcohol, every day 3 times, altogether replace 3 days, obtain pure silica wet gel microballoon.Supercritical Ethanol device is adopted to carry out drying to Wet Gel Microsphere;
(4) preparation of aerogel heat-proof coating: adopt the fatty acid methyl ester Soxylat A 25-7 FMEE of 0.015g as tensio-active agent, by dispersion agent, the wetting agent of it and 0.01g, the auxiliary agent such as defoamer, flow agent adds in 20g epoxy resin latex, stir, then add the silica aerosil microballoon 5g of modification, stir, add 0.01g thickening material adjusting viscosity, stir 3 minutes, at room temperature dry solidification three days, obtains aerosil thermal insulating coating;
(5) adopt Hot disk TPS 2500S thermal conductivity coefficient measurement instrument to detect thermal conductivity, the thermal conductivity of silica aerosil microballoon thermal insulating coating is 0.06980 W/ (mK).
Claims (8)
1. hydrophobic silica aerogel thermal insulating coating, primarily of polymer emulsion, hydrophobic silica aerogel microballoon and auxiliary agent composition, with the addition of tensio-active agent simultaneously.
2. hydrophobic silica aerogel thermal insulating coating according to claim 1, it is characterized in that a large amount of hydrophobic grouping is all contained in the surface of the silica aerosil microballoon adopted and inside, whole microballoon has complete hydrophobicity.
3. hydrophobic silica aerogel thermal insulating coating according to claim 1, key is the hydrophobically modified to silica aerosil microballoon, the present invention proposes two kinds of methods, first the first prepare silica wet gel microballoon, then be that properties-correcting agent carries out hydrophobically modified to silica wet gel microballoon with halogenated silanes, the second prepares the initial stage at colloidal sol, with the preparation for properties-correcting agent participation colloidal sol of organoalkoxysilane, silazane or siloxanes, finally obtain hydrophobic silica aerosil microballoon.
4. hydrophobic silica aerogel according to claim 3, when it is characterized in that silica aerosil microballoon modification, properties-correcting agent used is one or more in halogenated silanes, organoalkoxysilane, silazane or siloxanes.
5. hydrophobic silica aerogel according to claim 3, it is characterized in that halogenated silanes uses after silica wet gel microballoon completes, organoalkoxysilane, silazane or siloxanes use in silicon dioxide gel preparation process.
6. hydrophobic silica aerogel thermal insulating coating according to claim 1, is characterized in that have employed tensio-active agent.
7. tensio-active agent according to claim 6, is characterized in that tensio-active agent is polymer dielectric class, one or more in inorganic polymeric alkali salt class and high molecular polymer class.
8. hydrophobic silica aerogel thermal insulating coating according to claim 1, it is characterized in that polymer emulsion accounts for 10% ~ 95% of coating cumulative volume, the volume fraction of silica aerosil microballoon accounts for 5% ~ 90%, surfactant content is 0.1 ‰ ~ 5 ‰ of coating total mass, and other auxiliary agent sums are no more than 2 ‰ of coating quality.
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