CN103333542A - Silica aerogel microsphere composite thermal insulation coating - Google Patents
Silica aerogel microsphere composite thermal insulation coating Download PDFInfo
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- CN103333542A CN103333542A CN2013102776510A CN201310277651A CN103333542A CN 103333542 A CN103333542 A CN 103333542A CN 2013102776510 A CN2013102776510 A CN 2013102776510A CN 201310277651 A CN201310277651 A CN 201310277651A CN 103333542 A CN103333542 A CN 103333542A
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Abstract
The invention discloses a novel composite thermal insulation coating using silica aerogel microsphere as a thermal insulation filler. The main preparation process is as follows: mixing self-made silica aerogel microspheres with a polymer emulsion to obtain a silica aerogel composite thermal insulation coating with excellent heat insulation property. Compared with the existing coating in the market, the silica aerogel composite thermal insulation coating has greatly improved the thermal insulation property. The invention employs an atomization method to prepare the silica aerogel microspheres of micron size level, which have high filling rate of up to 70% in the coating. During the atomization process, the size of the silica aerogel microspheres is regulated by controlling the size of a nozzle. The invention also provides a method for preparing thermal insulation coating from silica aerogel microspheres with mixed grain size. Mixture of silica aerogel microspheres with different particle sizes is helpful to improving packing density of the silica aerogel microspheres in the coating, so as to reduce thermal conductivity of the coating to the minimum.
Description
Technical field
The present invention relates to a kind of is the novel heat-insulation coating of functional stuffing with the aerosil.Aerosil is a kind of have unique nanoporous and novel heat insulation material of tridimensional network, and this material thermal conductivity is extremely low, the effect of heat insulation excellence.Aerosil is a bold trial in heat insulation field as the use of thermal insulating filling, and it can significantly improve the heat-proof quality of existing thermal insulating coating, improves efficiency of energy utilization.Aerosil compound heat-insulation coating not only thermal insulation is good, and light-weight environment-friendly is nuisanceless, is comprising building, military affairs, and numerous areas such as space flight have huge potential using value.
Background technology
Along with the development of Chinese society, various places buildings emerge in multitude, the energy-saving and emission-reduction of interior of building outside become the focus that people pay close attention to day by day.Because the irradiation of sunlight, the temperature of interior of building can raise along with the prolongation of time, must cause the energy consumption of air-conditioning to increase like this.Simultaneously, factory, metal roof is adopted in temporary buildings such as movable dwellings more, under solar radiation, temperature raises very fast, adopts the poor effect of air-conditioning temperature-reducing, in order to improve this situation, the temperature that adopts a kind of thermal insulating coating efficiently to reduce building surface is a kind of practicable method.
Based on above reason, people begin to seek a kind of new and effective lagging material.Application at present is comparatively extensive, and what effect of heat insulation was best is the thermal insulating coating of the microballon filling of a class hollow structure.
Hollow beads is to include cavity, and the outer wall composition is the spheroid of the silicate of metal oxide such as ferro-aluminum calcium, owing to spherically have a minimum specific surface area, easily slide between sphere, thereby can reduce the consumption of base-material, and reduce the viscosity of coating, improve levelling property and the smoothness of filming.Hollow structure has reduced its thermal conductivity, and outer wall materials has opacifying property.Hollow beads commonly used has glass microballon, ceramic fine bead and float pearl.
Hollow glass microbead cheap, manufacture craft is simple, and therefore the reflectivity height becomes and uses maximum class hollow beads; The sealing thermal conductivity N little than air in the ceramic fine bead cavity
2And CO
2Deng gas, its outer wall materials is high temperature resistant, corrosion-resistant, thermal expansivity is little, but ceramic fine bead preparation technology is very complicated, cost is high, and is expensive, package stability is poor; Float pearl and be the microballon of a kind of hollow structure that the fine coal waste residue of thermal power plant produces in the process of cooling in air, the more artificial glass microballon of its price and ceramic fine bead are all low.
Added the thermal insulating coating of hollow beads, than existing thermal insulating coating on the market, effect of heat insulation improves a lot, and coating maximum heat conductance can reach about 0.1 W/ (mk).
Compare with above three kinds of lagging materials, aerosil is a kind of novel lagging material.Aerosil has nanoporous and three-dimensional netted skeleton structure, and density is little, and the aperture is little, porosity height, plurality of advantages such as specific surface area is big, and thermal conductivity is low, and it is strong, anti-oxidant also to have adsorptivity simultaneously, corrosion-resistant.Wherein thermal conductivity is low is the outstanding feature of aerosil.The inner a large amount of nanoporous of aerosil has limited the collision between the gas molecule, making gas molecule be similar to is adsorbed on the nanometer hole wall, thereby reduced gas phase heat conduction and the transmission of heat by convection of aerogel inside, made the thermal conductivity of aerosil descend greatly.In this different materials, the thermal conductivity of aerosil is minimum, and heat-proof quality is best.The thermal conductivity of different materials commonly used sees Table 1.
The thermal conductivity of table 1 lagging material commonly used
[0009]For the minimum thermal conductivity that detected silica aerogel heat-proof coating can reach, the present invention thinks that to aerosil content the thermal conductivity of thermal insulating coating detects.Detected result is seen accompanying drawing.Known that by accompanying drawing 1 the I of the thermal conductivity of coating reaches about 0.05W/ (mk).This shows that the aerosil thermal insulating coating is a kind of thermal insulating coating efficiently.
The main preparation technology of aerosil compound heat-insulation coating is divided into two steps: on the one hand by prepared aerosil microballoons such as sol-gel method and atomizations, on the other hand with the aerosil microballoon that makes and other emulsion, filler, auxiliary agent mixes, and prepares final compound heat-insulation coating.Because the block aerosil exists filling insufficient, therefore the defective of recycling etc. is used and often aerosil is prepared into micron-sized powder, to increase the range of application of aerosil.The form of silicon dioxide aerogel powder has multiple, and is bar-shaped as laminar, triangular shape etc., and this is that preparation method by aerogel powder determines.It is spheroidal that this paper adopts the silicon dioxide aerogel powder of atomization technique preparation, and micron order is compared the silicon dioxide aerogel powder of other forms, good dispersity, and good in the fillibility of coating, its filling ratio can be up to 70%.
Aerosil microballoon compound heat-insulation coating is a kind of novel heat insulation material.Compare with thermal insulating coating in the past, the aerosil microballoon has following advantage as thermal insulating filling:
1. the thermal conductivity of aerosil own is little, can improve the heat-proof quality of coating;
2. aerosil belongs to light porous material, and particle diameter is in micron order, and its filling ratio height in coating can greatly improve the thermal insulation of coating;
3. the aerosil microballoon is mano-porous material, and density is more much smaller than hollow beads, free settling not in coating;
4. earth silicon material, acid-alkali-corrosive-resisting, by hydrophobically modified, the water tolerance of aerogel microball improves, and adds in the coating good weatherability, long service life.
Summary of the invention
The invention provides a kind of is the major function filler with the aerosil, the novel heat-insulation coating of other color stuffing preparations of having mixed simultaneously.Main purpose is to seek a kind of heat-proof quality excellence by the matched combined of various fillers, and ultimate compression strength is big, and is anti-oxidant, anticorrosive, a kind of novel heat insulation material of long service life.
The technical solution used in the present invention is as follows:
With tetraethoxy (TEOS) and dehydrated alcohol (Ethanol), deionized water stirs after mixing, add nitric acid then and mix stirring, raw materials used mol ratio is TEOS:Ethanol: deionized water: nitric acid=1:0～15:1～10:0.0005～0.08 places water-bath with mixing solutions then, more than the insulation 1h, obtain silicon dioxide gel; Adopt spraying gun that silicon dioxide gel is sprayed in the oil phase, guarantee in the atomization process that oil phase has the rotating speed of 500r/min～1000r/min.The selected oil phase that atomizes is for the wet gel microballoon evenly being spread out, guaranteeing during atomizing that the sol volume in the oil phase is no more than 1/5 of oil phase volume.After atomizing is finished, add ammoniacal liquor in mixing solutions, ammonia volume is to begin to produce gel in the mixed solution to be as the criterion, and at room temperature aging two days, obtains the silica wet gel microballoon.The silica wet gel microballoon is filtered, and the elimination oil phase adopts remaining oil phase and the organic impurity of normal hexane displacement, replaces normal hexane with dehydrated alcohol then, obtains pure silica wet gel microballoon; With trimethylchlorosilane wet gel is carried out hydrophobic treatment; To through adding the mixing solutions of deionized water and dehydrated alcohol in the wet gel microballoon after the hydrophobic treatment, clean the foreign ion after modification is handled; In the wet gel microballoon, add dehydrated alcohol, replace wherein deionized water; The wet gel microballoon is carried out drying, obtain dry pure aerosil microballoon;
Calculate and take by weighing the emulsion of certain mass, aerosil microballoon and other fillers and auxiliary agent, auxiliary agent is added in the polymer emulsion, stir, in mixed solution, add aerosil microballoon and corresponding other auxiliary packings (as titanium dioxide, talcum powder etc.) again, stir, add thickening material and regulate viscosity, obtain aerosil compound heat-insulation coating.Wherein, each components contents (massfraction) is as follows: emulsion, 10%～95%; The aerosil microballoon, 10%～25%; Other auxiliary packings, 0～30%; Each analog assistant, 0.01%～0.3%.
The used aerosil of the present invention is micron order spherical shape nanoporous light material, and spherical complete, the microballoon size is seen accompanying drawing 2 between 1～300 μ m.
The present invention adopts atomization to prepare the aerosil microballoon, can control the size of aerogel microball by the diameter that changes used nozzle.Different in view of the coating thermal conductivity of the coating thermal conductivity of mixing the particle diameter preparation and single particle size preparation, a kind of method that particle diameter prepares the aerosil thermal insulating coating of mixing is provided simultaneously.The preparation method of aerosil microballoon is as described in technical scheme.Difference is, adopts the nozzle of two or more different diameters to atomize respectively during atomizing, for example 0.1mm and 0.5mm or 0.1mm, the nozzle of 0.3mm and 0.5mm.The aerogel microball of each nozzle preparation mixed according to a certain percentage when thermal insulating coating prepared, mix according to mass ratio 7:3 with the microballoon that the 0.5mm nozzle obtains as the microballoon that the 0.1mm nozzle is obtained, then mixed microballoon and emulsion are mixed with the aerosil thermal insulating coating.By the proportioning between the different ratios, can increase aerogel microball in the tap density of coating inside, make the thermal conductivity of coating drop to minimum.
Little (0.1～the 0.3g/cm of aerosil density that the present invention is prepared
3), porosity height (80%～99.8%), the big (600～1000m of specific surface area
2/ g), the aperture be nano level (1～80nm), median size little (5～250 μ m).The aerosil microballoon itself has good thermal insulation, and its thermal conductivity is after testing at 0.005～0.03W/ (mk). because the aerosil microballoon is in micron order, particle diameter is very little, so it can abundant stuffed heat insulated coating.Its volume fraction at coating can reach more than 80%, and the thermal conductivity of adding aerogel itself is extremely low, and this makes the thermal conductivity of aerosil thermal insulating coating can reach a mnm..
The present invention is water-borne coatings, and used binding agent comprises pure-acrylic emulsion, benzene emulsion, all kinds of emulsions such as organosilicon crylic acid latex and Resins, epoxy, acrylic resin, urethane etc.This class binding agent mainly contains high molecular polymer and water is mixed with, and viscosity is good after solidifying, and is good film forming matter.Can utilize homemade emulsion in addition, the thermal insulating coating that preparation has special purpose is as the photocuring thermal insulating coating etc.
It also can be several combinations that auxiliary packing among the present invention can be a kind of.Except the aerosil microballoon as the main thermal insulating filling.The effect of other fillers mainly is to promote physics and the mechanical property of coating, has excellent optical as titanium dioxide, the specific refractory power height, and light scattering ability is strong, and it is added coating, can increase the opacifying power of coating; Volumetric shrinkage when talcum powder can not only reduce paint solidification, the wear resistance of raising coating, cohesiveness reduces cost, and can also make coating have satisfactory stability and thermotolerance; The ash calcium powder can improve water tolerance and the moisture-proof pattern of fever of coating as active filler, adds the coating good leveling property of ash charge calcium powder, the slippery feel of filming.
Used auxiliary agent among the present invention, as wetting agent, dispersion agent, flow agent, defoamers etc. are commercially available.
The beneficial effect of the thermal insulating coating that the present invention is prepared:
The aerosil microballoon is light porous material, density is little, thermal conductivity is extremely low, and the volume content in coating can reach 60%, by the aerogel compound heat-insulation coating of its preparation, compare the market like product, heat-proof quality increases substantially, and be used for the surface of buildings with it summer, can effectively stop the temperature of building surface to rise, have certain insulation effect, reached effective purpose of energy saving.Aerosil compound heat-insulation coating application is convenient, and good weatherability is applicable to various complex environments.
Description of drawings
Fig. 1 is that the coating thermal conductivity is with SiO-
2The change curve of aerogel content;
Fig. 2 is the optical microscopy map of aerosil microballoon.
Embodiment
Example 1
With tetraethoxy (TEOS) and dehydrated alcohol (Ethanol), deionized water stirs after mixing, add nitric acid then and mix stirring, raw materials used mol ratio is TEOS:Ethanol: deionized water: nitric acid=1:0～15:1～10:0.0005～0.08 places water-bath with mixing solutions then, more than the insulation 1h, obtain silicon dioxide gel; Adopt spraying gun that silicon dioxide gel is sprayed in the oil phase, atomizer nozzle diameter 0.1mm guarantees in the atomization process that oil phase has the rotating speed of 500r/min～1000r/min.The selected oil phase that atomizes is for the wet gel microballoon evenly being spread out, guaranteeing during atomizing that the sol volume in the oil phase is no more than 1/5 of oil phase volume.After atomizing is finished, add ammoniacal liquor in mixing solutions, ammonia volume is to begin to produce gel in the mixed solution to be as the criterion, and at room temperature aging two days, obtains the silica wet gel microballoon.The silica wet gel microballoon is filtered, the elimination oil phase, adopt remaining oil phase and the organic impurity of normal hexane displacement, normal hexane consumption 550ml handles four every day, carried out altogether three days, replace normal hexane with dehydrated alcohol then, obtain pure silica wet gel microballoon, dehydrated alcohol consumption 500ml, handle every day three times, carried out altogether four days; With trimethylchlorosilane wet gel is carried out hydrophobic treatment, the each 20ml of trimethylchlorosilane consumption, two days hydrophobic treatment once, hydrophobic 6 days altogether; To through adding the mixing solutions of deionized water and dehydrated alcohol in the wet gel microballoon after the hydrophobic treatment, clean the foreign ion after modification is handled, the volume ratio of deionized water and dehydrated alcohol is 1:1, cumulative volume 500ml cleans three every day, cleans altogether three days; Add dehydrated alcohol in the wet gel microballoon, replace wherein deionized water, ethanol volume 150ml cleans three every day, cleans altogether four days; Adopt the Supercritical Ethanol device that the wet gel microballoon is carried out drying, obtain dry pure aerosil microballoon.
With dispersant B YK180, wetting agent PE100, auxiliary agents such as defoamer Foamaser50, organosilicon flow agent add in the 20g pure-acrylic emulsion, stir, the aerosil microballoon 6g that adds modification in the mixed solution, add titanium dioxide 2.89g, stir, add the thickening material Natvosol and regulate viscosity, obtain the aerosil thermal insulating coating, auxiliary agent content is 0.01g.
Detect through thermal conductivity, the thermal conductivity minimum is 0.068W/ (mk).Added after the titanium dioxide, painting color obviously bleaches, and opacifying power rises.
Example 2
With tetraethoxy (TEOS) and dehydrated alcohol (Ethanol), deionized water stirs after mixing, add nitric acid then and mix stirring, raw materials used mol ratio is TEOS:Ethanol: deionized water: nitric acid=1:0～15:1～10:0.0005～0.08 places water-bath with mixing solutions then, more than the insulation 1h, obtain silicon dioxide gel; Adopt spraying gun that silicon dioxide gel is sprayed in the oil phase, adopt the nozzle of diameter 0.1mm and the nozzle of diameter 0.3mm to atomize during atomizing respectively, guarantee in the atomization process that oil phase has the rotating speed of 500r/min～1000r/min.The selected oil phase that atomizes is for the wet gel microballoon evenly being spread out, guaranteeing during atomizing that the sol volume in the oil phase is no more than 1/5 of oil phase volume.After atomizing is finished, add ammoniacal liquor in mixing solutions, ammonia volume is to begin to produce gel in the mixed solution to be as the criterion, and at room temperature aging two days, obtains the silica wet gel microballoon.The silica wet gel microballoon is filtered, the elimination oil phase, adopt remaining oil phase and the organic impurity of normal hexane displacement, replace normal hexane with dehydrated alcohol then, obtain pure silica wet gel microballoon and with trimethylchlorosilane wet gel is carried out hydrophobic treatment, the each 20ml of trimethylchlorosilane consumption, two days hydrophobic treatment once, hydrophobic 6 days altogether; To through adding the mixing solutions of deionized water and dehydrated alcohol in the wet gel microballoon after the hydrophobic treatment, clean the foreign ion after modification is handled, the volume ratio of deionized water and dehydrated alcohol is 1:1, cumulative volume 500ml cleans three every day, cleans altogether three days; Add dehydrated alcohol in the wet gel microballoon, replace wherein deionized water, ethanol volume 150ml cleans three every day, cleans altogether four days; Adopt the Supercritical Ethanol device that the wet gel microballoon is carried out drying, obtain dry pure aerosil microballoon.
With dispersion agent Sn5040, wetting agent Wet991, defoamer Sn345, flow agent TB120 adds in the 30g epoxy resin latex, auxiliary agent content is 0.01g, stir, the aerosil microballoon 9g and the talcum powder that add modification in the mixed solution, when the aerosil microballoon added, with the 0.1mm nozzle, the aerosil microballoon of 0.3mm nozzle and the preparation of 0.5 nozzle mixed, mass ratio is 6:3:1, stir, add the rheology modified thickening material RM2020 of 0.01g urethane and regulate viscosity, stirred 3 minutes, add 3g solidifying agent phthalic anhydride, stir, at room temperature dry solidification is three days, obtains the aerosil thermal insulating coating.It is 0.076 W/ (mk) that thermal conductivity detects the thermal conductivity that shows coating minimum.
Example 3
With 208g tetraethoxy (TEOS) and 322g dehydrated alcohol (Ethanol), the 72g deionized water stirs after mixing, and adds 1ml2w% nitric acid then and mixes stirring, then mixing solutions is placed water-bath, more than the insulation 1h, obtain silicon dioxide gel; Adopt spraying gun that silicon dioxide gel is sprayed in the oil phase, atomizer nozzle diameter 0.1mm guarantees in the atomization process that oil phase has the rotating speed of 500r/min～1000r/min.The selected oil phase that atomizes is for the wet gel microballoon evenly being spread out, guaranteeing during atomizing that the sol volume in the oil phase is no more than 1/5 of oil phase volume.After atomizing is finished, add ammoniacal liquor in mixing solutions, ammonia volume is to begin to produce gel in the mixed solution to be as the criterion, and at room temperature aging two days, obtains the silica wet gel microballoon.The silica wet gel microballoon is filtered, the elimination oil phase, adopt remaining oil phase and the organic impurity of normal hexane displacement, the each consumption 200ml of normal hexane handles 3 every day, carried out altogether 3 days, replace normal hexane with dehydrated alcohol then, the ethanol consumption is 250ml, handles every day 3 times, carried out altogether 3 days, and obtained pure silica wet gel microballoon; With trimethylchlorosilane wet gel is carried out hydrophobic treatment, the each 20ml of trimethylchlorosilane consumption, two days hydrophobic treatment once, hydrophobic 6 days altogether; To through adding the mixing solutions of deionized water and dehydrated alcohol in the wet gel microballoon after the hydrophobic treatment, clean the foreign ion after modification is handled, the volume ratio of deionized water and dehydrated alcohol is 1:1, cumulative volume 500ml cleans three every day, cleans altogether three days; Add dehydrated alcohol in the wet gel microballoon, replace wherein deionized water, ethanol volume 150ml cleans three every day, cleans altogether four days; Adopt the Supercritical Ethanol device that the wet gel microballoon is carried out drying, obtain dry pure aerosil microballoon.
Polyester polyol, isophorone diisocyanate are carried out processed, add catalyzer dibutyl tin laurate, hydrophilic chain extender dihydroxypropionic acid and glycol ether again and react 4～5h down at 70～80 ℃, drip the Propylene glycol monoacrylate that is dissolved with hydroquinone of polymerization retarder in will reacting then and carry out end capping 2～3h, reaction process adds the viscosity of small amount of acetone conditioned reaction system, reaction is cooled to the neutralization of the triethylamine of adding below 50 ℃, make water-based UV polyurethane acrylate prepolymer.Polyester polyol: isophorone diisocyanate: dihydroxypropionic acid: glycol ether: hydroxy acrylate=0.75:2.4:0.6:0.4:1.6, catalyzer and hydroquinone of polymerization retarder are respectively 0.5% and 0.2% of system total mass.
Get 20g water-based UV polyurethane acrylate prepolymer, to the dispersant B YK180 that wherein adds 0.01g respectively, wetting agent PE100, auxiliary agents such as defoamer Sn345, flow agent TB120, stir, add aerosil microballoon 4g again, stir, add light trigger Dard2 cur1173 then, thinner M500 stirs, and static froth breaking namely gets aerosil compound heat-insulation coating.
Detect to show that this coating set time in the sun is 2～3 hours, thermal conductivity is minimum to be 0.06 W/ (mk), is suitable for the automatic assembly line application of factory.
Claims (7)
1. adopt sol-gel method and atomization to prepare the aerosil microballoon, then polymeric binder is mixed with the aerosil microballoon, add a little auxiliary simultaneously and prepared the aerosil compound heat-insulation coating with good effect of heat insulation, in addition, in order to improve the physical and mechanical property of coating, added some auxiliary packings, the over-all properties of coating is optimized.
2. aerosil compound heat-insulation coating according to claim 1 is characterized in that adopting aerosil microballoon conduct thermal insulating filling wherein, and aerogel microball is the micron order spherical particle, sphere diameter 1 ~ 300 μ m.
3. aerosil compound heat-insulation coating according to claim 1 is characterized in that adopting the aerosil microballoon of different-grain diameter to carry out proportioning preparation mixing particle diameter filler, to improve the tap density of microballoon in coating.
4. the aerosil microballoon of different-grain diameter according to claim 3 is characterized in that used nozzle diameter when changing atomizing is simultaneously regulated and control the size of aerosil microballoon by the atomization preparation.
5. aerosil compound heat-insulation coating according to claim 1, it is characterized in that adopting high molecular polymer is binding agent, and polymkeric substance wherein is Resins, epoxy, pure-acrylic emulsion, benzene emulsions etc. also can adopt the heat insulation coating that has both with other performances of self-control emulsion preparation in addition.
6. aerosil compound heat-insulation coating according to claim 1 is characterized in that adding some auxiliary packings, comprises talcum powder, titanium dioxide, calcium carbonate, wollastonite powder, barium sulfate, mica powder, pure aluminium silicate, calcium sulfate, calcium hydroxide, flyash, one or more in the polypropylene fibre.
7. aerosil compound heat-insulation coating according to claim 1, the quality that it is characterized in that polymer emulsion accounts for 10%～95% of coating total mass, the aerogel microball quality accounts for 10%～25%, and other fillers account for 0～30%, auxiliary agent content sum 0.01%～0.3%.
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